反応式
C([O:8][C:9]1[CH:26]=[CH:25][C:12]([O:13][C:14]2[C:23]([CH3:24])=[N:22][C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[N:15]=2)=[CH:11][CH:10]=1)C1C=CC=CC=1.O>C(Cl)Cl>[OH:8][C:9]1[CH:10]=[CH:11][C:12]([O:13][C:14]2[C:23]([CH3:24])=[N:22][C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[N:15]=2)=[CH:25][CH:26]=1参加物
4
実験手順
A solution of 12.5 g (0.05 mole) borontribromide in 100 cc methylene chloride was added, over a period of 40 minutes, to a well stirred, cold (-62° C.) solution of 17.1 g 2-(4-benzyloxyphenoxy)-3-methylquinoxaline (0.05 mole) in 400 cc methylene chloride. When the addition was complete, the temperature of the reaction was allowed to rise slowly (2 hours) to room temperature. The reaction mixture was then poured into 1 liter of water and an additional 500 cc of methylene chloride was added. The mixture was stirred vigorously for 40 minutes and the insoluble solid was filtered. Crystallization from an ethanol-water mixture (1:1) gave 6.4 g of product, m.p. 175°-178° C.
後処理
- additionWhen the addition
- custom(2 hours)
- customto room temperature
- stirringThe mixture was stirred vigorously for 40 minutes
- filtrationthe insoluble solid was filtered
- customCrystallization from an ethanol-water mixture (1:1)
出典と根拠
- ORDレコード
- ord-2e50a64fef51404880287fa09ec46d4f
- 出典データセット
- uspto-grants-1986_09
- 特許番号
- US04609396
関連ノート
読み込み中…