Chloroacetonitrile → 2-[(3R)-3-carbamoyloxypyrrolidin-1-yl]-2-iminoethylchloride hydrochloride

HRID 622410노트

반응식

HRID 622410 반응식
[Cl:1][CH2:2][C:3]#[N:4].[Na].Cl.[C:7]([O:10][C@@H:11]1[CH2:15][CH2:14][NH:13][CH2:12]1)(=[O:9])[NH2:8]>CO>[ClH:1].[C:7]([O:10][C@@H:11]1[CH2:15][CH2:14][N:13]([C:3](=[NH:4])[CH2:2][Cl:1])[CH2:12]1)(=[O:9])[NH2:8]

참가 물질

5

반응물 3

HCID 7856ChloroacetonitrileHCID 5360545SodiumHCID 67938211(3R)-3-carbamoyloxypyrrolidine hydrochloride

생성물 1

HCID 679383042-[(3R)-3-carbamoyloxypyrrolidin-1-yl]-2-iminoethylchloride hydrochloride

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

0.646 ml of chloroacetonitrile was added to a solution of 23 mg of metallic sodium in 8 ml of absolute methanol, the mixture was stirred for about 60 minutes at room temperature, 1.70 g of (3R)-3-carbamoyloxypyrrolidine hydrochloride were then added, and the mixture was stirred for a further 3 hours. After completion of the reaction, a small amount of insoluble material was filtered off and the solvent was stripped off from the filtrate. Ether was added to the residue, and the precipitated crystals were collected by filtration and washed with ether, giving 2.20 g of 2-[(3R)-3-carbamoyloxypyrrolidin-1-yl]-2-iminoethylchloride hydrochloride.

후처리

  1. stirringthe mixture was stirred for a further 3 hours
  2. customAfter completion of the reaction
  3. filtrationa small amount of insoluble material was filtered off
  4. additionEther was added to the residue
  5. filtrationthe precipitated crystals were collected by filtration
  6. washwashed with ether

출처 및 근거

ORD 기록
ord-8a89dfa2177840be8b6a02aa98006288
출처 데이터셋
uspto-grants-1988_09
특허 번호
US04771046

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