Diphenylcyclopropenone → HCID 21462217、化合物
反応式
[C:1]1([C:7]2[C:9](=[O:10])[C:8]=2[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:17]([C:19]1[CH:20]=[N:21][CH:22]=[CH:23][C:24]=1[C:25]#[N:26])#[N:18]>ClC1C=CC=CC=1>[OH:10][C:9]1[C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[C:8]([C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=2)[N:21]2[C:22]=1[CH:23]=[C:24]([C:25]#[N:26])[C:19]([C:17]#[N:18])=[CH:20]2参加物
4
実験手順
Diphenylcyclopropenone (0.319 g, 1.55 mmol) and 3,4-dicyanopyridine (0.200 g, 1.55 mmol) were mixed in a dry, argon filled reaction flask. Chlorobenzene (2.5 mL) (oxygen free) was added, and the reaction was heated to 130C. After 2 h the heating was stopped and the reaction was allowed to reach room temperature. Petroleum ether 40-60C (2.5 mL) was added in order to obtain a complete precipitate of the product. The solvent was filtered off and the precipitate was washed with petroleum ether. The crude product was stirred with chloroform (30. mL) for lb. The dark chloroform solution was filtered off leaving the title product as a yellow precipitate.
後処理
- additionfilled
- customreaction flask
- customto reach room temperature
- customto obtain a complete precipitate of the product
- filtrationThe solvent was filtered off
- washthe precipitate was washed with petroleum ether
- filtrationThe dark chloroform solution was filtered off
出典と根拠
- ORDレコード
- ord-2bd5c21322c742cfb57ecb786c08207f
- 出典データセット
- uspto-grants-1995_07
- 特許番号
- US05435991
反応ノート
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