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

Triethylamine → HCID 19370295, 화합물

HRID 129756
노트
인쇄 미리보기

반응식

HRID 129756 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[CH2:6]([O:8][C:9]([N:11]([CH2:13][CH2:14][OH:15])[CH3:12])=[O:10])[CH3:7].C(N(CC)CC)C>C(Cl)Cl>[CH3:1][S:2]([O:15][CH2:14][CH2:13][N:11]([C:9]([O:8][CH2:6][CH3:7])=[O:10])[CH3:12])(=[O:4])=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 19370355ethyl N-(2-hydroxyethyl)-N-methylcarbamate

생성물 1

HCID 19370295HCID 19370295, 화합물수율 103.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1.65 g of methanesulfonyl chloride was added dropwise, with stirring, to a solution of 1.66 g of 2-(N-ethoxycarbonyl-N-methylamino)ethanol and 1.65 g of triethylamine in 20 ml of methylene chloride, whilst ice-cooling, and the solution was then stirred at the same temperature for 30 minutes. At the end of this time, the mixture was poured into ice-water and extracted with methylene chloride. The extracts were combined and washed with water, after which they were dried over anhydrous sodium sulfate. Evaporation of the solvent under reduced pressure gave a residue which was purified by column chromatography through silica gel, using a 2:1 by volume mixture of ethyl acetate and hexane as the eluent, to give 2.62 g (yield 81%) of the title compound as an oil.

후처리

  1. temperaturecooling
  2. extractionextracted with methylene chloride
  3. washwashed with water
  4. dry with materialafter which they were dried over anhydrous sodium sulfate
  5. customEvaporation of the solvent under reduced pressure
  6. customgave a residue which
  7. customwas purified by column chromatography through silica gel
  8. additionby volume mixture of ethyl acetate and hexane as the eluent

출처 및 근거

ORD 기록
ord-d7fbf0c63ccd48629c71ca48031e669e
출처 데이터셋
uspto-grants-1995_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05470851

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트