홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

4,5-Dihydro-2-(methylthio)thiazole → (4R)-4,5-Dihydro-2-(methylthio)-4-thiazolemethanol

HRID 1957384
노트
인쇄 미리보기

반응식

HRID 1957384 반응식
[C:1](=[O:4])([O-])O.[K+].[CH3:6][S:7][C:8]1[S:9][CH2:10][CH2:11][N:12]=1>>[OH:4][CH2:1][C@@H:11]1[CH2:10][S:9][C:8]([S:7][CH3:6])=[N:12]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 883244,5-Dihydro-2-(methylthio)thiazoleHCID 516893Potassium Bicarbonate2회

생성물 1

HCID 22862349(4R)-4,5-Dihydro-2-(methylthio)-4-thiazolemethanol수율 99.2%

실험 절차

To a 73 ml solution of methanol anhydride containing 7.95 g of 3-hydroxyazetidine hydrochloride (5) obtained in the above Example 3, there was added 5.09 g of potassium hydrogencarbonate at a room temperature, and, then, there was added 9.67 g of 2-(methylthio)-1,3-thiazoline dropwise, and, then, the resultant solution was subjected to heating and reflux for 20 hours. After the reaction liquid was left still until it had a room temperature, 3.63 g of potassium hydrogencarbonate was further added, and the liquid was stirred for one hour at the same temperature. After the reaction was over, precipitate was removed by filtration, and the solvent was evaporated in a vacuum, and, to the obtained residue, there was added 100 ml of tetrahydrofuran, and the resulting mixture was stirred for one hour at a room temperature. Insoluble matters were removed by filtration, and the solvent was evaporated in a vacuum, and, then, the residue was subjected to silica gel column chromatography (eluent: chloroform-methanol), and, thus, there was obtained 8.23 g (yield: 71.5%) of 3-hydroxy-1-(1,3-thiazolin-2-yl)azetidine (6) in the form of colorless crystal.

후처리

  1. temperatureto heating
  2. temperaturereflux for 20 hours
  3. customAfter the reaction liquid
  4. waitwas left still until it
  5. customhad a room temperature
  6. customwas removed by filtration
  7. customthe solvent was evaporated in a vacuum
  8. additionto the obtained residue, there was added 100 ml of tetrahydrofuran
  9. stirringthe resulting mixture was stirred for one hour at a room temperature
  10. customInsoluble matters were removed by filtration
  11. customthe solvent was evaporated in a vacuum

출처 및 근거

ORD 기록
ord-37d7c8607cce4d08884099827dc5568a
출처 데이터셋
uspto-grants-1998_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05783703

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트