4-Methylbenzoyl Chloride → 5-(4-Toluamido)-3-Trichloromethyl-1,2,4-Thiadiazole

HRID 66937

反応式

HRID 66937 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.[C:11]1([CH3:20])[CH:16]=[CH:15][C:14]([C:17](Cl)=[O:18])=[CH:13][CH:12]=1>C1(C)C=CC=CC=1>[C:11]1([CH3:20])[CH:16]=[CH:15][C:14]([C:17]([NH:1][C:2]2[S:6][N:5]=[C:4]([C:7]([Cl:10])([Cl:9])[Cl:8])[N:3]=2)=[O:18])=[CH:13][CH:12]=1

参加物

4

反応物 2

HCID 134054-Methylbenzoyl ChlorideHCID 6028483-(Trichloromethyl)-1,2,4-thiadiazol-5-amine

生成物 1

HCID 130415165-(4-Toluamido)-3-Trichloromethyl-1,2,4-Thiadiazole

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A solution of 11.0 g (0.05 mole) 5-amino-3-trichloromethyl-1,2,4-thiadiazole and 8.0 g (0.05 mole) 4-toluoyl chloride in 250 ml toluene was heated at reflux for 20 hours. Unreacted amino compound was removed by cooling the reaction mixture and filtering the precipitate. Concentration of the filtrate in vacuo gave the crude product, which was purified by recrystallization from cyclohexane. Yield was 9.1 g (27%); m.p. 127° C.

後処理

  1. temperatureat reflux for 20 hours
  2. customUnreacted amino compound was removed
  3. temperatureby cooling the reaction mixture
  4. filtrationfiltering the precipitate

出典と根拠

ORDレコード
ord-941fe4c55371425b876f0a5cbd9052c1
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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