反応式
[CH2:1]([O:8][C:9]1[CH:27]=[CH:26][C:25]([Br:28])=[CH:24][C:10]=1[CH2:11][N:12]([C:15]1[CH:20]=[CH:19][C:18]([C:21]([OH:23])=O)=[CH:17][N:16]=1)[CH2:13][CH3:14])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:29]([S:32]([NH2:35])(=[O:34])=[O:33])[CH2:30][CH3:31].CN(C1N=CC=CN=1)C.Cl.CN(C)CCCC(N=C=N)C.Cl>ClCCl>[CH2:1]([O:8][C:9]1[CH:27]=[CH:26][C:25]([Br:28])=[CH:24][C:10]=1[CH2:11][N:12]([C:15]1[CH:20]=[CH:19][C:18]([C:21]([NH:35][S:32]([CH2:29][CH2:30][CH3:31])(=[O:34])=[O:33])=[O:23])=[CH:17][N:16]=1)[CH2:13][CH3:14])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1参加物
7
反応物 5
生成物 1
試薬・触媒・溶媒 1
実験手順
To a solution of 2-(N-(2-benzyloxy-5-bromobenzyl)-N-ethylamino]pyridine-5-carboxylic acid (0.89 g) in dichloromethane (50 ml) was added propanesulphonamide (0.3 g), dimethylaminopyrimidine (0.493 g) and 1-(3-dimethylaminopropyl)ethylcarbodiimide hydrochloride (0.58 g). The mixture was stirred at ambient temperature for 18 hours, and poured into 2N HCl. The organic layer was separated and washed with water and brine, then dried (MgSO4), filtered and evaporated. The resulting oil was purified by chromatography on silica gel (eluting with 5% ethylacetate/dichloromethane to give N-(2-[N-(2-benzyloxy-5-bromobenzyl)-N-ethylamino]pyridine-5-carbonyl)propanesulphonamide (271 mg) as a white foam.
後処理
- customThe organic layer was separated
- washwashed with water and brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- customevaporated
- customThe resulting oil was purified by chromatography on silica gel (
- washeluting with 5% ethylacetate/dichloromethane
出典と根拠
- ORDレコード
- ord-8c64db4ba7724ab8abb4c242bc02427f
- 出典データセット
- uspto-grants-1998_12
- 特許番号
- US05843942
関連ノート
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