Itaconic acid → 1-Cyclohexyl-5-oxopyrrolidine-3-carboxylic acid

HRID 58554

반응식

HRID 58554 반응식
[CH:1]1([NH2:7])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH2:8]=[C:9]([CH2:13][C:14](O)=[O:15])[C:10]([OH:12])=[O:11].[OH-].[Na+]>O>[CH:1]1([N:7]2[C:14](=[O:15])[CH2:13][CH:9]([C:10]([OH:12])=[O:11])[CH2:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

참가 물질

5

반응물 3

HCID 811Itaconic acidHCID 7965CyclohexylamineHCID 14798Sodium Hydroxide

생성물 1

HCID 2385461-Cyclohexyl-5-oxopyrrolidine-3-carboxylic acid수율 58.1%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
110 °C

실험 절차

A mixture of cyclohexanamine (3.70 mL; 31.94 mmol) and 2-methylenesuccinic acid (5.04 g; 41.62 mmol) in water (10 mL) was heated in a sealed tube at 110° C. for 21 hours. After cooling to room temperature, 6N NaOH (10 mL) was added and the resulting precipitate was filtered off. The filtrate was acidified with 6N hydrochloric acid to pH 1 and the resulting precipitate was filtered, washed with water, and dried to yield 3.92 g (58%) of 1-cyclohexyl-5-oxopyrrolidine-3-carboxylic acid as a white solid.

후처리

  1. temperatureAfter cooling to room temperature
  2. filtrationthe resulting precipitate was filtered off
  3. filtrationthe resulting precipitate was filtered
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-f89a7a3e2ec1406fb3da65e56c726d6c
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09434722B2

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