反応 #1375807

反応方程式

intermediate 7-a

2- [(4-chlorophenyl)(1-methyl-1H-benzotriazol-6-yl)methyl]hydrazinecarboxaldehyde

methanimidamide monoacetate

water

→

(+)-6-[(4-chlorophenyl)-(1H-1,2,4-triazol-1-yl)methyl]-1-methyl-1H-benzotriazole

収率 67.1%

溶媒

methanol

反応条件

後処理

1. 1
   温度was refluxed for 3 days
2. 2
   その他To the warm reaction mixture there
3. 3
   ろ過The precipitate was filtered off
4. 4
   洗浄washed with 2-propanol
5. 5
   その他The precipitate was dried in vacuo

実験手順

A mixture of 5 g of intermediate 7-a, 8.2 g of methanimidamide monoacetate in 32 ml of methanol was refluxed for 3 days. To the warm reaction mixture there were added 32 ml of water and the resulting mixture was stirred for two hours. The precipitate was filtered off and washed with 2-propanol. The precipitate was dried in vacuo, yielding 3.45 g (67%) of (+)-6-[(4-chlorophenyl)-(1H-1,2,4-triazol-1-yl)methyl]-1-methyl-1H-benzotriazole (comp. 1-e); enantiomeric excess: 97.4%.

出典