3-bromopiperidin-4-one;hydrobromide

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 4.55 g thiourea was added to 15.2 g 3-Bromo-piperidin-4-one hydrobromide in 152 mL ethanol and refluxed for 20 h. The reaction was cooled and the solid was filtered, washed with ethanol and dried to give 15.8 g of the desired product. refluxed for 20 h The reaction was cooled the solid was filtered washed with ethanol dried

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 4.7 mL 33% HBr in acetic acid, 11.4 g bromine in 30 mL acetic acid was added slowly to a stirred solution of 10 g piperidine-4,4-diol in 60 mL acetic acid at RT. The reaction mixture was stirred additional 45 min at ambient temperature and the acetic acid was completely removed under reduced pressure. The residue was dissolved in 200 mL acetone and refluxed for 1 hour, cooled, filtered and washed with acetone and dried to give 15.2 g of the desired product the acetic acid was completely removed under reduced pressure The residue was dissolved in 200 mL acetone refluxed for 1 hour cooled filtered washed with acetone dried

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 4.55 g thiourea was added to 15.2 g 3-Bromo-piperidin-4-one hydrobromide in 152 mL ethanol and refluxed for 20 h. The reaction was cooled and the solid was filtered, washed with ethanol and dried to give 15.8 g of the desired product., (M+H)+: 184 refluxed for 20 h The reaction was cooled the solid was filtered washed with ethanol dried

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 4.7 mL 33% HBr in acetic acid and 11.4 g bromine in 30 mL acetic acid were added slowly to a stirred solution of 10 g piperidin-4-one in 60 mL acetic acid at RT. The reaction mixture was stirred for additional 45 min at ambient temperature and the acetic acid was completely removed under reduced pressure. The residue was dissolved in 200 mL acetone and refluxed for 1 h, cooled, filtered and washed with acetone and dried to give 15.2 g of the desired product, (M+H)+: 180. the acetic acid was completely removed under reduced pressure The residue was dissolved in 200 mL acetone refluxed for 1 h cooled filtered washed with acetone dried

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 4.55 g thiourea was added to 15.2 g 3-Bromo-piperidin-4-one hydrobromide in 152 mL ethanol and refluxed for 20 h. The reaction was cooled and the solid was filtered, washed with ethanol and dried to give 15.8 g of the desired product. refluxed for 20 h The reaction was cooled the solid was filtered washed with ethanol dried

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 4.7 mL 33% HBr in acetic acid, 11.4 g bromine in 30 mL acetic acid was added slowly to a stirred solution of 10 g piperidine-4,4-diol in 60 mL acetic acid at RT. The reaction mixture was stirred additional 45 min at ambient temperature and the acetic acid was completely removed under reduced pressure. The residue was dissolved in 200 mL acetone and refluxed for 1 hour, cooled, filtered and washed with acetone and dried to give 15.2 g of the desired product the acetic acid was completely removed under reduced pressure The residue was dissolved in 200 mL acetone refluxed for 1 hour cooled filtered washed with acetone dried

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 4.7 mL 33% HBr in acetic acid, 11.4 g bromine in 30 mL acetic acid was added slowly to a stirred solution of 10 g piperidine-4,4-diol in 60 mL acetic acid at RT. The reaction mixture was stirred additional 45 min at ambient temperature and the acetic acid was completely removed under reduced pressure. The residue was dissolved in 200 mL acetone and refluxed for 1 hour, cooled, filtered and washed with acetone and dried to give 15.2 g of the desired product the acetic acid was completely removed under reduced pressure The residue was dissolved in 200 mL acetone refluxed for 1 hour cooled filtered washed with acetone dried

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 4.55 g thiourea was added to 15.2 g 3-Bromo-piperidin-4-one hydrobromide in 152 mL ethanol and refluxed for 20 h. The reaction was cooled and the solid was filtered, washed with ethanol and dried to give 15.8 g of the desired product., (M+H)+: 184 refluxed for 20 h The reaction was cooled the solid was filtered washed with ethanol dried

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 4.7 mL 33% HBr in acetic acid and 11.4 g bromine in 30 mL acetic acid were added slowly to a stirred solution of 10 g piperidin-4-one in 60 mL acetic acid at RT. The reaction mixture was stirred for additional 45 min at ambient temperature and the acetic acid was completely removed under reduced pressure. The residue was dissolved in 200 mL acetone and refluxed for 1 h, cooled, filtered and washed with acetone and dried to give 15.2 g of the desired product, (M+H)+: 180. the acetic acid was completely removed under reduced pressure The residue was dissolved in 200 mL acetone refluxed for 1 h cooled filtered washed with acetone dried

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: About 2.6 g of N-butoxycarbonyl-4-piperdone (FIG. 10b) was dissolved in about 70 ml of chloroform; to this solution was added about 2.08 g Br2 over a period of about 30 minutes. The reaction was continued for about 2 hours at room temperature during which a white precipitate of the compound of FIG. 10c was formed. The reaction mixture was filtered and washed with chloroform ether to yield about 2.76 g of the compound of FIG. 10c. a white precipitate of the compound of FIG. 10c was formed The reaction mixture was filtered washed with chloroform ether

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: About 2.6 g of N-butoxycarbonyl-4-piperdone (FIG. 10b) was dissolved in about 70 ml of chloroform; to this solution was added about 2.08 g Br2 over a period of about 30 minutes. The reaction was continued for about 2 hours at room temperature during which a white precipitate of the compound of FIG. 10c was formed. The reaction mixture was filtered and washed with chloroform ether to yield about 2.76 g of the compound of FIG. 10c. a white precipitate of the compound of FIG. 10c was formed The reaction mixture was filtered washed with chloroform ether

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: About 2.6 g of N-butoxycarbonyl-4-piperdone (FIG. 10b) was dissolved in about 70 ml of chloroform; to this solution was added about 2.08 g Br2 over a period of about 30 minutes. The reaction was continued for about 2 hours at room temperature during which a white precipitate of the compound of FIG. 10c was formed. The reaction mixture was filtered and washed with chloroform ether to yield about 2.76 g of the compound of FIG. 10c. a white precipitate of the compound of FIG. 10c was formed The reaction mixture was filtered washed with chloroform ether