Ethyl (chloroformyl)acetate → Ethyl 2-(trifluoromethyl)-1,3-thiazole-5-carboxylate

HRID 1781588

反応式

HRID 1781588 の反応式
[F:1][C:2]([F:7])([F:6])[C:3]([NH2:5])=[S:4].Cl[CH:9]([CH:15]=O)[C:10]([O:12][CH2:13][CH3:14])=[O:11]>ClCCl>[F:1][C:2]([F:7])([F:6])[C:3]1[S:4][C:9]([C:10]([O:12][CH2:13][CH3:14])=[O:11])=[CH:15][N:5]=1

参加物

4

反応物 2

HCID 118030Ethyl (chloroformyl)acetateHCID 4425751Trifluoroethanethioamide

生成物 1

HCID 15171126Ethyl 2-(trifluoromethyl)-1,3-thiazole-5-carboxylate収率 24.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
70 °C

実験手順

A mixture of 11.22 g of 2,2,2,-trifluorothioacetamide and 10.14 g of ethyl 2-chloro-2-formylacetate was stirred for 30 minutes in an oil bath of 70° C. and then for 1.5 hours in an oil bath of 100° C., to which 100 ml of dichloromethane were added. After removing an insoluble substance, the mixture was concentrated and the residue was subjected to a column chromatography [developing solvent: hexane-ethyl acetate (10:1)], to obtain 3.74 g of ethyl 2-(trifluoromethyl)-5-thiazolecarboxylate as yellow liquid.

後処理

  1. waitfor 1.5 hours in an oil bath of 100° C.
  2. customAfter removing an insoluble substance
  3. concentrationthe mixture was concentrated

出典と根拠

ORDレコード
ord-e77115f6fff944f5b5d1ed887385f92e
出典データセット
uspto-grants-1997_05
特許番号
US05633375

関連ノート

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