Methylamine → HCID 68784750、化合物
反応式
[CH3:1][NH2:2].[CH:3]1[C:11]2[C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[S:8][C:7]=2[CH:6]=[CH:5][C:4]=1[S:16](Cl)(=[O:18])=[O:17]>S1(CCCC1)(=O)=O.O>[CH3:1][NH:2][S:16]([C:4]1[CH:5]=[CH:6][C:7]2[S:8][C:9]3[CH:15]=[CH:14][CH:13]=[CH:12][C:10]=3[C:11]=2[CH:3]=1)(=[O:18])=[O:17]参加物
5
実験手順
A large excess of aqueous methylamine was added to a suspension of dibenzo[b,d]thiophene-2-sulfonyl chloride (2.83 g) in sulfolane (15 ml) and the mixture was stirred at RT for 3 h. The reaction mixture was diluted with water, and the precipitate was recovered, washed with water, dried and purified by silica gel chromatography eluting with a gradient of ethyl acetate:DCM of 0:100 to 10:90 to give the title compound (1.79 g, 64%).
後処理
- customthe precipitate was recovered
- washwashed with water
- customdried
- custompurified by silica gel chromatography
- washeluting with a gradient of ethyl acetate
出典と根拠
- ORDレコード
- ord-15911a9013df404bbfe80b2581b3c8f7
- 出典データセット
- uspto-grants-2015_09
- 特許番号
- US09145380B2
反応ノート
読み込み中…