反応式
[NH2:1][C:2]1[CH:23]=[CH:22][C:5]([C:6]([N:8]2[C:14]3[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=3[CH2:12][N:11]3[CH:19]=[CH:20][CH:21]=[C:10]3[CH2:9]2)=[O:7])=[CH:4][C:3]=1[O:24][CH3:25].C(N(CC)CC)C.[CH2:33]([S:37](Cl)(=[O:39])=[O:38])[CH2:34][CH2:35][CH3:36]>C(Cl)Cl>[CH3:25][O:24][C:3]1[CH:4]=[C:5]([CH:22]=[CH:23][C:2]=1[NH:1][S:37]([CH2:33][CH2:34][CH2:35][CH3:36])(=[O:39])=[O:38])[C:6]([N:8]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[CH2:12][N:11]2[CH:19]=[CH:20][CH:21]=[C:10]2[CH2:9]1)=[O:7]参加物
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
To a stirred solution of 0.10 g of 10,11-dihydro-10-(4-amino-3-methoxybenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine in 2 ml of methylene chloride is added 60 mg of triethylamine followed by a solution of 56 mg of n-butylsulfonyl chloride in 0.5 ml of methylene chloride. After stirring at room temperature for 2 hours, the reaction mixture is evaporated in vacuo to a residue which is dissolved in methyl alcohol, stirred for 1 hour and evaporated in vacuo to a residue which is treated with 2 ml of NH4Cl and extracted with 15 ml of ethyl acetate. The organic extract is washed with saturated NaHCO3, brine, dried Na2SO4), filtered through hydrous magnesium silicate and the filtrate evaporated to a residue. The residue is stirred with ether-hexanes to give 0.14 g of light yellow solid. MS (CI ): 454 (M+H).
後処理
- customthe reaction mixture is evaporated in vacuo to a residue which
- dissolutionis dissolved in methyl alcohol
- stirringstirred for 1 hour
- customevaporated in vacuo to a residue which
- additionis treated with 2 ml of NH4Cl
- extractionextracted with 15 ml of ethyl acetate
- extractionThe organic extract
- washis washed with saturated NaHCO3, brine, dried Na2SO4),
- filtrationfiltered through hydrous magnesium silicate
- customthe filtrate evaporated to a residue
- stirringThe residue is stirred with ether-hexanes
出典と根拠
- ORDレコード
- ord-5c224e4471b6449891596267f1ea9940
- 出典データセット
- uspto-grants-1996_05
- 特許番号
- US05516774
関連ノート
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