Hydrochloric Acid → 2-(3-Methoxyiminopyrrolidin-1-yl)-2-iminoethylmercaptan hydrochloride

HRID 622420노트

반응식

HRID 622420 반응식
P(=[S:5])([O-])([O-])[O-].[Na+].[Na+].[Na+].Cl.[CH3:10][O:11][N:12]=[C:13]1[CH2:17][CH2:16][N:15]([C:18](=[NH:21])[CH2:19][Cl:20])[CH2:14]1.Cl>O>[ClH:20].[CH3:10][O:11][N:12]=[C:13]1[CH2:17][CH2:16][N:15]([C:18](=[NH:21])[CH2:19][SH:5])[CH2:14]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 9877537Trisodium thiophosphateHCID 867424272-(3-Methoxyiminopyrrolidin-1-yl)-2-iminoethylchloride hydrochloride

생성물 1

HCID 867424292-(3-Methoxyiminopyrrolidin-1-yl)-2-iminoethylmercaptan hydrochloride수율 77%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

1.77 g of trisodium phosphorothioate were added to an ice-cooled solution of 2.1 g of 2-(3-methoxyiminopyrrolidin-1-yl)-2-iminoethylchloride hydrochloride in 12 ml of water, and the mixture was stirred at room temperature for about one hour. 9.8 ml of 1N hydrochloric acid were then added, and the mixture was heated at 65° C. for 30 minutes. The resulting solution was concentrated under reduced pressure, the concentrate was mixed with 9.8 ml of isopropanol, insolubles were filtered off, and the filtrate was concentrated under reduced pressure. Ether was added to the concentrate, and the crystals which separated out were collected by filtration and reprecipitated from a mixture of ethanol and ether, giving 1.6 g of 2-(3-methoxyiminopyrrolidin-1-yl)-2-iminoethylmercaptan hydrochloride.

후처리

  1. temperaturethe mixture was heated at 65° C. for 30 minutes
  2. concentrationThe resulting solution was concentrated under reduced pressure
  3. additionthe concentrate was mixed with 9.8 ml of isopropanol, insolubles
  4. filtrationwere filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. additionEther was added to the concentrate
  7. customthe crystals which separated out
  8. filtrationwere collected by filtration
  9. customreprecipitated from a mixture of ethanol and ether

출처 및 근거

ORD 기록
ord-561924d555e245bea9c6b81c156da4be
출처 데이터셋
uspto-grants-1988_09
특허 번호
US04771046

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