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

HRID 725003노트

반응식

HRID 725003 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 2.2-2.5(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-095f3b197e044ad49d2a696423a78f70
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05705516

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