1-benzyl 3-Methyl pyrrolidine-1,3-dicarboxylate synthesis
- Product Name:1-benzyl 3-Methyl pyrrolidine-1,3-dicarboxylate
- CAS Number:912444-75-8
- Molecular formula:C14H17NO4
- Molecular Weight:263.29
912444-74-7
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Yield:912444-75-8 99%
Reaction Conditions:
Stage #1: 1-benzyl 3-methyl 3-methylpyrrolidine-1,3-dicarboxylatewith water;lithium hydroxide in ethanol; for 1 h;Heating;
Stage #2: with potassium hydrogensulfate in water; pH=3 - 4;
Steps:
D.C
[00255] Step C: A 3M LiOH solution (14.7 mL, 29.4 mmol) was added to 1-benzyl 3- methyl 3-methylpyrrolidine-l,3-dicarboxylate (2.72 g, 9.81 mmol) in ethanol (15 mL), and the reaction mixture was stirred at 78°C (bath) for 1 hour. The ethanol was removed, and ether (30 mL) was added. The aqueous layer was separated and acidified with saturated potassium hydrogen sulfate to a pH of about 3 to about 4, extracted with ethyl acetate (50 mL), washed with brine and dried over sodium sulfate. After removal of the solvent, l-(benzyloxycarbonyl)-3- methylpyrrolidine-3-carboxylic acid (2.56 g, 99% yield) was isolated as an oil.
References:
WO2009/140320,2009,A1 Location in patent:Page/Page column 74
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912444-75-8
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912444-75-8
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912444-75-8
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912444-75-8
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