反応式
O=[C:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[S:6][C:5]2[CH:13]=[CH:14][CH:15]=[CH:16][C:4]=2[NH:3]1.B.CSC.CO>O1CCCC1>[CH:9]1[C:8]2[CH2:2][NH:3][C:4]3[CH:16]=[CH:15][CH:14]=[CH:13][C:5]=3[S:6][C:7]=2[CH:12]=[CH:11][CH:10]=1参加物
5
実験手順
To a mixture of 3.3 g of 10,11-dihydro-11-oxodibenz[b,f][1,4]thiazepine in 25 ml of tetrahydrofuran is added 4.0 ml of 10 molar borane-dimethylsulfide in tetrahydrofuran. The mixture is stirred at room temperature for 18 hours, 50 ml of anhydrous methanol added and the solvent removed. An additional 30 ml of methanol is added and the solvent removed to give white crystals. A sample is purified by chromatography on silica gel with hexane-chloroform-ethyl acetate (2:1:1) as solvent to give white crystals, m.p. 145°-148° C.
後処理
- customthe solvent removed
- additionAn additional 30 ml of methanol is added
- customthe solvent removed
- customto give white crystals
- customA sample is purified by chromatography on silica gel with hexane-chloroform-ethyl acetate (2:1:1) as solvent
- customto give white crystals, m.p. 145°-148° C.
出典と根拠
- ORDレコード
- ord-39c2414928ca4ba296ae3349d9d22d6f
- 出典データセット
- uspto-grants-1998_11
- 特許番号
- US05834461
関連ノート
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