3-benzylpiperazin-2-one

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

Procedure: Benzyl chloroformate (8.5 g.) is added to a stirred mixture of 3-(phenylmethyl)piperazinone (XXIX, Example 62, 6.8 g.), chloroform (75 ml.), and saturated sodium bicarbonate solution (20 ml.). After 30 minutes the chloroform phase is separated, washed twice with water, and concentrated. The residual oil is crystallized from ethyl acetate-SSB and then ethyl acetate again to give the title compound, m.p. 125°-127.5°. After 30 minutes the chloroform phase is separated washed twice with water concentrated The residual oil is crystallized from ethyl acetate-SSB

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

Procedure: Ethylenediamine (25 g.) is added to a stirred solution of ethyl 2-bromo-3-phenylpropionate (XXVII, Example 61, 14.0 g.) in THF (100 ml.) and ethanol (300 ml.). After 20 hours at 20°-25° the solvents are removed under reduced pressure and the residual oil is partitioned between ethyl acetate-1N sodium hydroxide solution. The ethyl acetate extract is washed with water, saline, and concentrated. The residual oil is applied to a silica gel column which is eluted with chloroform-methanol (9/1). Fractions containing the product are pooled, concentrated to a residue and recrystallized from ethyl acetate-SSB to give 3-(phenylmethyl)piperazinone, m.p. 92°-93°. After 20 hours at 20°-25° the solvents are removed under reduced pressure the residual oil is partitioned between ethyl acetate-1N sodium hydroxide solution The ethyl acetate extract is washed with water, saline concentrated is eluted with chloroform-methanol (9/1) Fractions containing the product concentrated to a residue recrystallized from ethyl acetate-SSB

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

Procedure: Benzyl chloroformate (8.5 g.) is added to a stirred mixture of 3-(phenylmethyl)piperazinone (XXIX, Example 62, 6.8 g.), chloroform (75 ml.), and saturated sodium bicarbonate solution (20 ml.). After 30 minutes the chloroform phase is separated, washed twice with water, and concentrated. The residual oil is crystallized from ethyl acetate-SSB and then ethyl acetate again to give the title compound, m.p. 125°-127.5°. After 30 minutes the chloroform phase is separated washed twice with water concentrated The residual oil is crystallized from ethyl acetate-SSB

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

Procedure: Ethylenediamine (25 g.) is added to a stirred solution of ethyl 2-bromo-3-phenylpropionate (XXVII, Example 61, 14.0 g.) in THF (100 ml.) and ethanol (300 ml.). After 20 hours at 20°-25° the solvents are removed under reduced pressure and the residual oil is partitioned between ethyl acetate-1N sodium hydroxide solution. The ethyl acetate extract is washed with water, saline, and concentrated. The residual oil is applied to a silica gel column which is eluted with chloroform-methanol (9/1). Fractions containing the product are pooled, concentrated to a residue and recrystallized from ethyl acetate-SSB to give 3-(phenylmethyl)piperazinone, m.p. 92°-93°. After 20 hours at 20°-25° the solvents are removed under reduced pressure the residual oil is partitioned between ethyl acetate-1N sodium hydroxide solution The ethyl acetate extract is washed with water, saline concentrated is eluted with chloroform-methanol (9/1) Fractions containing the product concentrated to a residue recrystallized from ethyl acetate-SSB

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

Procedure: Benzyl chloroformate (8.5 g.) is added to a stirred mixture of 3-(phenylmethyl)piperazinone (XXIX, Example 62, 6.8 g.), chloroform (75 ml.), and saturated sodium bicarbonate solution (20 ml.). After 30 minutes the chloroform phase is separated, washed twice with water, and concentrated. The residual oil is crystallized from ethyl acetate-SSB and then ethyl acetate again to give the title compound, m.p. 125°-127.5°. After 30 minutes the chloroform phase is separated washed twice with water concentrated The residual oil is crystallized from ethyl acetate-SSB

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

Procedure: Ethylenediamine (25 g.) is added to a stirred solution of ethyl 2-bromo-3-phenylpropionate (XXVII, Example 61, 4.0 g.) in THF (100 ml.) and ethanol (300 ml.). After 20 hours at 20°-25° the solvents are removed under reduced pressure and the residual oil is partitioned between ethyl acetate-1 N sodium hydroxide solution. The ethyl acetate extract is washed with water, saline, and concentrated. The residual oil is applied to a silica gel column which is eluted with chloroform-methanol (9/1). Fractions containing the product are pooled, concentrated to a residue and recrystallized from ethyl acetate-SSB to give 3-(phenylmethyl)piperazinone, m.p. 92°-93°. After 20 hours at 20°-25° the solvents are removed under reduced pressure the residual oil is partitioned between ethyl acetate-1 N sodium hydroxide solution The ethyl acetate extract is washed with water, saline concentrated is eluted with chloroform-methanol (9/1) Fractions containing the product concentrated to a residue recrystallized from ethyl acetate-SSB

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

Procedure: Benzyl chloroformate (8.5 g.) is added to a stirred mixture of 3-(phenylmethyl)piperazinone (XXIX, Example 62, 6.8 g.), chloroform (75 ml.), and saturated sodium bicarbonate solution (20 ml.). After 30 minutes the chloroform phase is separated, washed twice with water, and concentrated. The residual oil is crystallized from ethyl acetate-SSB and then ethyl acetate again to give the title compound, m.p. 125°-127.5°. After 30 minutes the chloroform phase is separated washed twice with water concentrated The residual oil is crystallized from ethyl acetate-SSB

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

Procedure: Ethylenediamine (25 g.) is added to a stirred solution of ethyl 2-bromo-3-phenylpropionate (XXVII, Example 61, 14.0 g.) in THF (100 ml.) and ethanol (300 ml.). After 20 hours at 20°-25° the solvents are removed under reduced pressure and the residual oil is partitioned between ethyl acetate-1N sodium hydroxide solution. The ethyl acetate extract is washed with water, saline, and concentrated. The residual oil is applied to a silica gel column which is eluted with chloroform-methanol (9/1). Fractions containing the product are pooled, concentrated to a residue and recrystallized from ethyl acetate-SSB to give 3-(phenylmethyl)piperazinone, m.p. 92°-93°. After 20 hours at 20°-25° the solvents are removed under reduced pressure the residual oil is partitioned between ethyl acetate-1N sodium hydroxide solution The ethyl acetate extract is washed with water, saline concentrated is eluted with chloroform-methanol (9/1) Fractions containing the product concentrated to a residue recrystallized from ethyl acetate-SSB