Sodium Hydroxide → (2S)-1-methyl-5-oxopyrrolidine-2-carboxylic acid

HRID 554112

반응식

HRID 554112 반응식
[CH3:1][N:2]1[C:11](=[O:12])[CH2:10][CH2:9][C@H:3]1[C:4]([O:6]CC)=[O:5].[OH-].[Na+]>C(O)C>[CH3:1][N:2]1[C:11](=[O:12])[CH2:10][CH2:9][C@H:3]1[C:4]([OH:6])=[O:5]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 15225832Ethyl 1-methyl-5-oxoprolinate

생성물 1

HCID 18649403(2S)-1-methyl-5-oxopyrrolidine-2-carboxylic acid

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
0 °C

실험 절차

Ethyl 1-methyl-5-oxoprolinate (0.27 g, 1.58 mmol) was dissolved in ethanol (5 ml) and cooled to 0° C. in an ice bath. To this was added 2M aqueous sodium hydroxide solution (3 ml) and the mixture was stirred for ˜4 hours at 0° C. The ethanol was evaporated under vacuum and the aqueous residue was acidified with 2N aqueous hydrogen chloride to pH1. The volume of the aqueous phase was reduced to ˜3 ml under vacuum and then extracted with a 3:1 mixture of chloroform and isopropanol using a phase separator. The combined organic layers were concentrated to give 1-methyl-5-oxoproline which was used without further purification.

후처리

  1. customThe ethanol was evaporated under vacuum
  2. extractionextracted with a 3:1 mixture of chloroform and isopropanol using a phase separator
  3. concentrationThe combined organic layers were concentrated

출처 및 근거

ORD 기록
ord-acfa93724bc2414eb4f16580866091d3
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08048907B2

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