3,5-Dinitrobenzoyl chloride → 5-(3,5-Dinitrobenzamido)-3-Trichloromethyl-1,2,4-Thiadiazole

HRID 66941

反応式

HRID 66941 の反応式
[NH2:1][C:2]1[S:6][N:5]=[C:4]([C:7]([Cl:10])([Cl:9])[Cl:8])[N:3]=1.[N+:11]([C:14]1[CH:15]=[C:16]([CH:20]=[C:21]([N+:23]([O-:25])=[O:24])[CH:22]=1)[C:17](Cl)=[O:18])([O-:13])=[O:12]>C1(C)C=CC=CC=1>[N+:11]([C:14]1[CH:15]=[C:16]([CH:20]=[C:21]([N+:23]([O-:25])=[O:24])[CH:22]=1)[C:17]([NH:1][C:2]1[S:6][N:5]=[C:4]([C:7]([Cl:10])([Cl:9])[Cl:8])[N:3]=1)=[O:18])([O-:13])=[O:12]

参加物

4

反応物 2

HCID 74323,5-Dinitrobenzoyl chlorideHCID 6028483-(Trichloromethyl)-1,2,4-thiadiazol-5-amine

生成物 1

HCID 130415205-(3,5-Dinitrobenzamido)-3-Trichloromethyl-1,2,4-Thiadiazole収率 85%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
-10 °C

実験手順

A solution of 10.9 g (0.05 mole) 5-amino-3-trichloromethyl-1,2,4-thiadiazole and 12.6 g (0.055 mole) 3,5-dinitrobenzoyl chloride in 200 ml toluene was refluxed for 20 hours. The crude product precipitated from the reaction mixture upon cooling to -10° C. After isolation by filtration, the residue was washed with hot petroleum ether and finally recrystallized from methylene chloride to give 17.5 g (85% yield) of pure product; m.p. 197° C.

後処理

  1. customThe crude product precipitated from the reaction mixture
  2. filtrationAfter isolation by filtration
  3. washthe residue was washed with hot petroleum ether
  4. customfinally recrystallized from methylene chloride

出典と根拠

ORDレコード
ord-8e93b465b8fa4b39bec5f67f154ba6ef
出典データセット
uspto-grants-1982_08
特許番号
US04343945

関連ノート

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