Potassium Carbonate → 2-(4-Bromo-3,4,4-trifluorobutylthio)thiazole

HRID 1416315노트

반응식

HRID 1416315 반응식
[SH:1][C:2]1[S:3][CH:4]=[CH:5][N:6]=1.[Br:7][C:8]([F:15])([F:14])[CH:9]([F:13])[CH2:10][CH2:11]Br.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[Br:7][C:8]([F:15])([F:14])[CH:9]([F:13])[CH2:10][CH2:11][S:1][C:2]1[S:3][CH:4]=[CH:5][N:6]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 27834041,4-Dibromo-1,1,2-trifluorobutaneHCID 178527881HCID 178527881, 화합물

생성물 1

HCID 218505172-(4-Bromo-3,4,4-trifluorobutylthio)thiazole수율 96.5%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

2-Mercaptothiazole (11.7 g) in acetone (30 cm3) containing 1,4-dibromo-1,1,2-trifluorobutane (27.0 g) was treated portionwise with anhydrous potassium carbonate (13.8 g) under an atmosphere of nitrogen. The reaction was stirred for 1.5 hours, filtered and the insolubles washed with further acetone (4×25 cm3). The filtrate was evaporated under reduced pressure and the residue fractionated by chromatography (silica, eluant 10% ethyl acetate in hexane) to give 2-(4-bromo-3,4,4-trifluorobutylthio)thiazole (29.5 g). 1H NMR: δ 22-2.5(2H,m); 3.2-3.6(2H,m); 4.7-5.0(1H,m); 7.23(1H,d); 7.68(1H,d).

후처리

  1. filtrationfiltered
  2. washthe insolubles washed with further acetone (4×25 cm3)
  3. customThe filtrate was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-8980ad2e62fd4c4493ced44f803e5710
출처 데이터셋
uspto-grants-1999_06
특허 번호
US05912243

반응 노트

불러오는 중…