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

HRID 591501

反応式

HRID 591501 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-efea65c911b44c3f9e75c2d061f7696b
出典データセット
uspto-grants-2016_01
特許番号
US09238639B2

関連ノート

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