三乙胺 → 6-Methyl-2-oxo-4-(phenylmethyl)-3-[[(phenylmethyl)sulphonyl]amino]-1,2-dihydropyridine-1acetic Acid
反应方程式
C(N(CC)CC)C.[C:8]1([CH2:14][S:15](Cl)(=[O:17])=[O:16])[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[NH2:19][C:20]1[C:21](=[O:39])[N:22]([CH2:34][C:35]([O:37]C)=[O:36])[C:23]([CH3:33])=[CH:24][C:25]=1[CH2:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1>ClCCl>[CH3:33][C:23]1[N:22]([CH2:34][C:35]([OH:37])=[O:36])[C:21](=[O:39])[C:20]([NH:19][S:15]([CH2:14][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)(=[O:17])=[O:16])=[C:25]([CH2:26][C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[CH:24]=1参与物
实验过程
1 ml (7.17 mmol) of triethylamine and 0.95 g (5 mmol) of (phenylmethyl)sulphonyl chloride are added to 1 g (3.5 mmol) of methyl 3-amino-6-methyl-2-oxo-4-(phenylmethyl)-1,2-dihydropyridine-1-acetate in solution in 30 ml of dichloromethane and the mixture is kept stirred for 12 hours at room temperature. The reaction medium is washed successively with 10 ml of water, 10 ml of a 1 N aqueous hydrochloric acid solution and then 10 ml of a saturated sodium chloride solution. The medium is dried over magnesium sulphate and evaporated. The residue is purified by chromatography on a silica gel column, eluting with a dichloromethane:methanol (98:2) mixture. The product is used as such in the hydrolysis stage which is carried out according to the procedure described in Example 3. 0.8 g of product is obtained in the form of a white powder.
后处理
- washThe reaction medium is washed successively with 10 ml of water, 10 ml of a 1 N aqueous hydrochloric acid solution
- dry with materialThe medium is dried over magnesium sulphate
- customevaporated
- customThe residue is purified by chromatography on a silica gel column
- washeluting with a dichloromethane:methanol (98:2) mixture
- customsuch in the hydrolysis stage which
来源与证据
- ORD记录
- ord-b6e2874a73304385b05b4d2a96caa06e
- 来源数据集
- uspto-grants-2001_06
- 专利号
- US06252082B1
反应笔记
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