Methanethioamide → HCID 13015600、化合物

HRID 1058348

反応式

HRID 1058348 の反応式
[CH:1]([NH2:3])=[S:2].[CH2:4]([O:6][C:7](=[O:15])[CH:8](Cl)[C:9](=O)[CH:10]([CH3:12])[CH3:11])[CH3:5]>C(O)C>[CH2:4]([O:6][C:7]([C:8]1[S:2][CH:1]=[N:3][C:9]=1[CH:10]([CH3:12])[CH3:11])=[O:15])[CH3:5]

参加物

4

反応物 2

HCID 3005587MethanethioamideHCID 9877606Ethyl 2-chloro-4-methyl-3-oxopentanoate

生成物 1

HCID 13015600HCID 13015600、化合物収率 36%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of thioformamide (prepared according to A1-Razzar et al. U.S. Pat, No. 5,559158; 1.2 g, 20 mmol) and 2-chloro-4-methyl-3-oxopentanoic acid ethyl ester (2.0 g, 10 mmol) in ethanol (20 mL) was heated at reflux for 17 h. The reaction mixture was evaporated to dryness and the residue was chromatographed over silica gel (5-20% ethyl acetate/hexanes) to give 4-(1-methylethyl)thiazole-5-carboxylic acid ethyl ester (720 mg, 36% yield).

後処理

  1. temperatureat reflux for 17 h
  2. customThe reaction mixture was evaporated to dryness
  3. customthe residue was chromatographed over silica gel (5-20% ethyl acetate/hexanes)

出典と根拠

ORDレコード
ord-129a30faf3f14682a1471b9b795211e5
出典データセット
uspto-grants-2003_02
特許番号
US06515124B2

関連ノート

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