1,3-Dichloroacetone → 4-(Chloromethyl)-2-(4-methylphenyl)-1,3-thiazole

HRID 538582

反応式

HRID 538582 の反応式
[Cl:1][CH2:2][C:3]([CH2:5]Cl)=O.[CH3:7][C:8]1[CH:16]=[CH:15][C:11]([C:12]([NH2:14])=[S:13])=[CH:10][CH:9]=1>C1(C)C=CC=CC=1>[Cl:1][CH2:2][C:3]1[N:14]=[C:12]([C:11]2[CH:15]=[CH:16][C:8]([CH3:7])=[CH:9][CH:10]=2)[S:13][CH:5]=1

参加物

4

反応物 2

HCID 107931,3-DichloroacetoneHCID 7372094-Methylbenzenecarbothioamide

生成物 1

HCID 20635964-(Chloromethyl)-2-(4-methylphenyl)-1,3-thiazole収率 67%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
120 °C

実験手順

To a solution of 1,3 dichloroacetone (0.84 g, 6.62 mmol) in toluene (5 ml) was added 4-methylthiobenzamide (0.50 g, 3.31 mmol) and the reaction mixture was heated at 120° C. for 1 h. After the completion of the reaction mixture (TLC monitoring), the reaction mixture was evaporated to dryness under reduced pressure and the residue was purified over silica gel (230-400 M, 15% EtOAc-Hexane) to get the desired product (0.49 g, 67%). The other derivatives were also prepared by the same general method.

後処理

  1. customAfter the completion of the reaction mixture (TLC monitoring), the reaction mixture was evaporated to dryness under reduced pressure
  2. customthe residue was purified over silica gel (230-400 M, 15% EtOAc-Hexane)

出典と根拠

ORDレコード
ord-4bdae525a99041d3b3ce866c47587deb
出典データセット
uspto-grants-2014_10
特許番号
US08865736B2

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