反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:10])[CH3:9])=[CH:4][C:3]=1[CH3:11].[CH3:12][S:13](Cl)(=[O:15])=[O:14]>N1C=CC=CC=1.O1CCCC1>[CH3:11][C:3]1[CH:4]=[C:5]([C:8](=[O:10])[CH3:9])[CH:6]=[CH:7][C:2]=1[NH:1][S:13]([CH3:12])(=[O:15])=[O:14]参加物
5
反応条件
- 温度
- 5 °C
実験手順
4'-Amino-3'-methylacetophenone from Step VIII (3.0 g, 20 mmol) in 15 ml of dry pyridine at 5° C. is reacted with 3.0 g (26.2 mmol) of methanesulfonyl chloride in 5 ml of tetrahydrofuran. The reaction is stirred at 5° C. for 2 hrs, then at room temperature overnight. The reaction is diluted with ice-water. The solid is collected, washed with water, air dried and crystallized from methylene chloride-pet. ether to yield the title compound; m.p. 152°-153° C.
後処理
- customat room temperature
- customovernight
- customThe solid is collected
- washwashed with water, air
- customdried
- customcrystallized from methylene chloride-pet. ether
出典と根拠
- ORDレコード
- ord-0ac4085aa85945ca8f78d814c4565448
- 出典データセット
- uspto-grants-1992_10
- 特許番号
- US05155268
関連ノート
読み込み中…