tert-Butanol → Ethyl 4-methyl-2-(trifluoromethyl)thiazole-5-carboxylate

HRID 591501

반응식

HRID 591501 반응식
[F:1][C:2]([F:7])([F:6])[C:3](=[S:5])[NH2:4].CC(O)(C)C.Cl[CH:14]([C:20](=O)[CH3:21])[C:15]([O:17][CH2:18][CH3:19])=[O:16]>CCOC(C)=O>[CH3:21][C:20]1[N:4]=[C:3]([C:2]([F:7])([F:6])[F:1])[S:5][C:14]=1[C:15]([O:17][CH2:18][CH3:19])=[O:16]

참가 물질

5

반응물 3

HCID 6386tert-ButanolHCID 11858Ethyl 2-chloroacetoacetateHCID 4425751Trifluoroethanethioamide

생성물 1

HCID 46835627Ethyl 4-methyl-2-(trifluoromethyl)thiazole-5-carboxylate

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a mixture of 2,2,2-trifluoroethanethioamide (200 mg) and t-BuOH (10 mL) was added ethyl 2-chloro-3-oxobutanoate (0.217 mL) at room temperature. The mixture was refluxed for 2 days. After cooling, EtOAc was poured into the mixture, and the mixture was washed successively with water and brine, dried over Na2SO4 and concentrated in vacuo. The residue was purified by silica gel column chromatography (NH, EtOAc/hexane) to give the title compound (133 mg).

후처리

  1. temperatureThe mixture was refluxed for 2 days
  2. temperatureAfter cooling
  3. washthe mixture was washed successively with water and brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by silica gel column chromatography (NH, EtOAc/hexane)

출처 및 근거

ORD 기록
ord-efea65c911b44c3f9e75c2d061f7696b
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09238639B2

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