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

HRID 622423노트

반응식

HRID 622423 반응식
P(=[S:5])([O-])([O-])[O-].[Na+].[Na+].[Na+].Cl.[OH:10][N:11]=[C:12]1[CH2:16][CH2:15][N:14]([C:17](=[NH:20])[CH2:18][Cl:19])[CH2:13]1.Cl>O>[ClH:19].[OH:10][N:11]=[C:12]1[CH2:16][CH2:15][N:14]([C:17](=[NH:20])[CH2:18][SH:5])[CH2:13]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 9877537Trisodium thiophosphateHCID 867424302-(3-Hydroxyiminopyrrolidin-1-yl)-2-iminoethylchloride hydrochloride

생성물 1

HCID 867424332-(3-Hydroxyiminopyrrolidin-1-yl)-2-iminoethylmercaptan hydrochloride수율 64.5%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

945 mg of trisodium phosphorothioate were added to a solution of 1.05 g of 2-(3-hydroxyiminopyrrolidin-1-yl)-2-iminoethylchloride hydrochloride in 6.4 ml of water, cooled with ice-water, and the mixture was stirred at room temperature for about one hour. 5.2 ml of 1N hydrochloric acid were added, and the mixture was heated at 65° C. for 30 minutes and then concentrated under reduced pressure. The concentrate was mixed with 5.2 ml of methanol, insolubles were filtered off, and the filtrate was concentrated under reduced pressure. Anhydrous ether was added to the concentrate, and the precipitated crystals were collected by filtration and washed with ether, giving 670 mg of 2-(3-hydroxyiminopyrrolidin-1-yl)-2-iminoethylmercaptan hydrochloride.

후처리

  1. temperaturethe mixture was heated at 65° C. for 30 minutes
  2. concentrationconcentrated under reduced pressure
  3. additionThe concentrate was mixed with 5.2 ml of methanol, insolubles
  4. filtrationwere filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. additionAnhydrous ether was added to the concentrate
  7. filtrationthe precipitated crystals were collected by filtration
  8. washwashed with ether

출처 및 근거

ORD 기록
ord-02014e8f7cfa476889b69de7191d4aee
출처 데이터셋
uspto-grants-1988_09
특허 번호
US04771046

반응 노트

불러오는 중…