2-CHLOROCARBONYL-2-METHYL-PROPIONIC ACID ETHYL ESTER

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

Procedure: To a solution of 61 g of N-methyl-β-alanine ethyl ester in 600 ml of dry pyridine there is added 82 g of ethyl 2-chloroformyl-2-methylpropionate. During the addition, which takes 30 minutes, the mixture is mechanically stirred and cooled with ice. Stirring is continued at 10° C for 30 minutes and then at 30° - 40° C for 1 hour. Next the pyridine is evaporated in vacuo, leaving a residue to which a small quantity of water is added, whereafter the mixture is extracted with ether. The extract is dried over magnesium sulphate and evaporated leaving the above-mentioned product as a liquid which is purified by distillation at reduced pressure. Yield 97 g (75%). Boiling point 134° - 136° C (1 mm). nD22 1.4565. During the addition, which cooled with ice Stirring is continued at 10° C for 30 minutes at 30° - 40° C for 1 hour Next the pyridine is evaporated in vacuo leaving a residue to which a small quantity of water is added, whereafter the mixture is extracted with ether The extract is dried over magnesium sulphate evaporated

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

Procedure: To a solution of 61 g of N-methyl-β-alanine ethyl ester in 600 ml of dry pyridine there is added 82 g of ethyl 2-chloroformyl-2-methylpropionate. During the addition, which takes 30 minutes, the mixture is mechanically stirred and cooled with ice. Stirring is continued at 10° C for 30 minutes and then at 30° - 40° C for 1 hour. Next the pyridine is evaporated in vacuo, leaving a residue to which a small quantity of water is added, whereafter the mixture is extracted with ether. The extract is dried over magnesium sulphate and evaporated leaving the above-mentioned product as a liquid which is purified by distillation at reduced pressure. Yield 97 g (75%). Boiling point 134° - 136° C (1 mm). nD22 1.4565. During the addition, which cooled with ice Stirring is continued at 10° C for 30 minutes at 30° - 40° C for 1 hour Next the pyridine is evaporated in vacuo leaving a residue to which a small quantity of water is added, whereafter the mixture is extracted with ether The extract is dried over magnesium sulphate evaporated

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

Procedure: To a solution of 61 g of N-methyl-β-alanine ethyl ester in 600 ml of dry pyridine there is added 82 g of ethyl 2-chloroformyl-2-methylpropionate. During the addition, which takes 30 minutes, the mixture is mechanically stirred and cooled with ice. Stirring is continued at 10° C for 30 minutes and then at 30° - 40° C for 1 hour. Next the pyridine is evaporated in vacuo, leaving a residue to which a small quantity of water is added, whereafter the mixture is extracted with ether. The extract is dried over magnesium sulphate and evaporated leaving the above-mentioned product as a liquid which is purified by distillation at reduced pressure. Yield 97 g (75%). Boiling point 134° - 136° C (1 mm). nD22 1.4565. During the addition, which cooled with ice Stirring is continued at 10° C for 30 minutes at 30° - 40° C for 1 hour Next the pyridine is evaporated in vacuo leaving a residue to which a small quantity of water is added, whereafter the mixture is extracted with ether The extract is dried over magnesium sulphate evaporated