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Ethyl bromopyruvate → Ethyl 2-(2,2,2-trifluoroethyl)thiazole-4-carboxylate

HRID 1689370
ノート
印刷プレビュー

反応式

HRID 1689370 の反応式
[F:1][C:2]([F:8])([F:7])[CH2:3][C:4](=[S:6])[NH2:5].Br[CH2:10][C:11](=O)[C:12]([O:14][CH2:15][CH3:16])=[O:13]>C1COCC1>[F:1][C:2]([F:8])([F:7])[CH2:3][C:4]1[S:6][CH:10]=[C:11]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[N:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 66144Ethyl bromopyruvateHCID 222204183,3,3-Trifluoropropanethioamide

生成物 1

HCID 57989344Ethyl 2-(2,2,2-trifluoroethyl)thiazole-4-carboxylate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 3,3,3-trifluoropropanethioamide (example 67, step b) (4 g) and ethyl 3-bromo-2-oxopropanoate (5.45 g) in THF (120 mL) was heated at reflux for 2 hours. The solvent was removed under reduced pressure and the residue was partitioned between ethyl acetate and saturated sodium bicarbonate solution. The organic layer was dried over sodium sulphate, filtered and the solvent evaporated under reduced pressure. The crude product was purified by flash silica chromatography using 17% ethyl acetate in isohexane as solvent. Pure fractions were evaporated to dryness to afford the subtitled compound. Yield 1.9 g.

後処理

  1. temperatureat reflux for 2 hours
  2. customThe solvent was removed under reduced pressure
  3. customthe residue was partitioned between ethyl acetate and saturated sodium bicarbonate solution
  4. dry with materialThe organic layer was dried over sodium sulphate
  5. filtrationfiltered
  6. customthe solvent evaporated under reduced pressure
  7. customThe crude product was purified by flash silica chromatography
  8. customPure fractions were evaporated to dryness

出典と根拠

ORDレコード
ord-1b437449f4b54487b9168ecc701e177d
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08148373B2

反応ノート

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