反応 #1375805

ord-a1244270bfea4e1b8f02a7b572c7861c

反応方程式

Cn1nnc2ccc(C(=O)c3ccc(Cl)cc3)cc21
(4-chlorophenyl)(1-methyl-1H-benzotriazole-6-yl)methanone
CC(C)(C)OC(=O)NN
1,1-dimethylethyl hydrazinecarboxylate
Cn1nnc2ccc(C(=NNC(=O)OC(C)(C)C)c3ccc(Cl)cc3)cc21
1,1-dimethylethyl [(4-chlorophenyl)(1 -methyl-1H-benzotriazol-6-yl)-methylene]hydrazine carboxylate
収率 59.2%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度at reflux temperature
  2. 2
    workup.STIRRINGstirring
  3. 3
    workup.WAITwas continued for 2 hours
  4. 4
    ろ過The precipitate was filtered off
  5. 5
    洗浄washed with ethanol
  6. 6
    その他dried in vacuo at 50° C.

実験手順

A mixture of 27.17 g of (4-chlorophenyl)(1-methyl-1H-benzotriazole-6-yl)methanone, 14.24 g of 1,1-dimethylethyl hydrazinecarboxylate and 80 ml of ethanol was stirred for 21 hours at reflux temperature. The reaction mixture was cooled to room temperature and stirring was continued for 2 hours. The precipitate was filtered off, washed with ethanol and dried in vacuo at 50° C., yielding 22.8 g (59.2%) of 1,1-dimethylethyl [(4-chlorophenyl)(1 -methyl-1H-benzotriazol-6-yl)-methylene]hydrazine carboxylate (interm. 1-b).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05746840uspto-grants-1998_05