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

Triethylamine → [2-Chloro-4-(trifluoromethyl)thiazol-5-yl]methyl methanesulfonate

HRID 354727
노트
인쇄 미리보기

반응식

HRID 354727 반응식
[Cl:1][C:2]1[S:3][C:4]([CH2:11][OH:12])=[C:5]([C:7]([F:10])([F:9])[F:8])[N:6]=1.C(N(CC)CC)C.[CH3:20][S:21](Cl)(=[O:23])=[O:22]>C1(C)C=CC=CC=1>[CH3:20][S:21]([O:12][CH2:11][C:4]1[S:3][C:2]([Cl:1])=[N:6][C:5]=1[C:7]([F:8])([F:9])[F:10])(=[O:23])=[O:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 12953359(2-Chloro-4-(trifluoromethyl)thiazol-5-yl)methanol

생성물 1

HCID 13106537[2-Chloro-4-(trifluoromethyl)thiazol-5-yl]methyl methanesulfonate수율 92%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a cold (0° C.) solution of 34.7 g (0.161 mol) of the compound of Example 4 in 150 ml of toluene there was added over a 30 minute period, 18.2 g (0.18 mol) of triethylamine. To this mixture was added 20.5 g (0.18 mol) of methanesulfonyl chloride. The reaction mixture was stirred at room temperature for 2 hours and was allowed to stand in the refrigerator for 4 days. The insoluble salt was filtered and the filtrate was concentrated under reduced pressure. The residue was dissolved in ether and the ether solution was washed with water, dried over MgSO4 and concentrated under reduced pressure to give 43.8 g (92%) of crude [2-chloro-4-(trifluoromethyl)thiazol-5-yl]methyl methanesulfonate. A 5.5 g portion of the crude material was dissolved in 50 ml of acetone. To this solution was added 2 g (0.0169 mol) of potassium xanthogenate. The reaction mixture was stirred for 2 hours at room temperature and filtered. The acetone filtrate was concentrated to give 6.9 g of oil which was chromatographed on silica gel using ether petroleum ether (1:9 v/v) as eluant. The earlier fraction was 4.1 g (69.9%) of S-[2-chloro-4-(trifluoromethyl)-5-thiazolyl]methyl O-ethyl carbonodithioate; nD25 1.5497-1.5517.

후처리

  1. waitto stand in the refrigerator for 4 days
  2. filtrationThe insoluble salt was filtered
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. dissolutionThe residue was dissolved in ether
  5. washthe ether solution was washed with water
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-f81c019924e34303998bc4b0b2bf149e
출처 데이터셋
uspto-grants-1983_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04377054

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트