反応式
C[O:2][C:3](=[O:40])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([C:12]2[N:17]=[C:16]([O:18][CH3:19])[C:15]([O:20][C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=3[O:27][CH3:28])=[C:14]([NH:29][S:30]([C:33]3[CH:38]=[CH:37][C:36]([CH3:39])=[CH:35][N:34]=3)(=[O:32])=[O:31])[N:13]=2)[CH:7]=1.[OH-].[Na+].C(Cl)Cl.CCOC(C)=O>CO>[CH3:19][O:18][C:16]1[C:15]([O:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=2[O:27][CH3:28])=[C:14]([NH:29][S:30]([C:33]2[CH:38]=[CH:37][C:36]([CH3:39])=[CH:35][N:34]=2)(=[O:32])=[O:31])[N:13]=[C:12]([C:8]2[CH:7]=[C:6]([CH:11]=[CH:10][CH:9]=2)[O:5][CH2:4][C:3]([OH:40])=[O:2])[N:17]=1参加物
5
実験手順
85 mg of {3-[4-methoxy-5-(2-methoxy-phenoxy)-6-(5-methyl-pyridine-2-sulfonylamino)-pyrimidin-2-yl]-phenoxy}-acetic acid methyl ester, product of example 2, dissolved in MeOH (30 ml) were treated at RT with 1N NaOH (0.9 ml) and the solution was stirred for 1 h until the transformation was complete according to TLC analysis (CH2Cl2/EtOAc: 3:1). The reaction mixture was partitioned between 1N HCl and CH2Cl2, the organic layer was dried over Na2SO4 and the solvent removed in vacuo. The residue upon triturating with ether provided the desired {3-[4-methoxy-5-(2-methoxy-phenoxy)-6-(5-methyl-pyridine-2-sulfonylamino)-pyrimidin-2-yl]-phenoxy}-acetic acid as a white solid. ISN mass spectrum, m/e 551 (M−1 calculated for C26H24N4O8S: 551).
後処理
- customThe reaction mixture was partitioned between 1N HCl and CH2Cl2
- dry with materialthe organic layer was dried over Na2SO4
- customthe solvent removed in vacuo
- customThe residue upon triturating with ether
出典と根拠
- ORDレコード
- ord-778690e5da974e81a54ca5de746623cc
- 出典データセット
- uspto-grants-2001_06
- 特許番号
- US06242601B1
関連ノート
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