Triethylamine → 1-Methylcarbamoyl-4-(3',5'-dichlorophenyl) urazole

HRID 371986ノート

反応式

HRID 371986 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[C:13](=[O:14])[NH:12][NH:11][C:10]2=[O:15])[CH:5]=[C:6]([Cl:8])[CH:7]=1.C(N(CC)CC)C.[CH3:23][N:24]=[C:25]=[O:26]>CN(C)C=O.O>[CH3:23][NH:24][C:25]([N:12]1[C:13](=[O:14])[N:9]([C:4]2[CH:3]=[C:2]([Cl:1])[CH:7]=[C:6]([Cl:8])[CH:5]=2)[C:10](=[O:15])[NH:11]1)=[O:26]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 12228Methyl IsocyanateHCID 187550094-(3,5-Dichlorophenyl)-1,2,4-triazolidine-3,5-dione

生成物 1

HCID 536345341-Methylcarbamoyl-4-(3',5'-dichlorophenyl) urazole

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 2.5 g of 4-(3',5'-dichlorophenyl) urazole in 10 ml of N,N-dimethylformamide were added a drop of triethylamine and, in turn, 0.8 g of methyl isocyanate dropwise at room temperature with agitation. The reaction was continued for one additional hour under the same conditions and the reaction mixture was poured in water to precipitate crystals which were filtered and recrystallized from acetoneethanol to obtain 1-methylcarbamoyl-4-(3',5'-dichlorophenyl) urazole in an amount of 2.1 g (yield being 68%).

後処理

  1. customdropwise at room temperature
  2. customto precipitate crystals which
  3. filtrationwere filtered
  4. customrecrystallized from acetoneethanol

出典と根拠

ORDレコード
ord-7e08e28a5ddb45e792dc145ae6ac7e1e
出典データセット
uspto-grants-1978_05
特許番号
US04088767

反応ノート

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