反応式
C(OC([N:6]1[CH2:9][C:8]([CH2:27][C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)([C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([O:16][CH2:17][CH2:18][NH:19][S:20]([CH2:23][CH:24]3[CH2:26][CH2:25]3)(=[O:22])=[O:21])[CH:11]=2)[CH2:7]1)=O)C.[OH-].[Na+].CCO>[Cl-].[Na+].O>[CH2:27]([C:8]1([C:10]2[CH:11]=[C:12]([CH:13]=[CH:14][CH:15]=2)[O:16][CH2:17][CH2:18][NH:19][S:20]([CH2:23][CH:24]2[CH2:25][CH2:26]2)(=[O:22])=[O:21])[CH2:7][NH:6][CH2:9]1)[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1参加物
4
反応物 2
生成物 1
試薬・触媒・溶媒 1
実験手順
To 3-benzyl-3-[3-(2-cyclopropylmethanesulfonylamino-ethoxy)-phenyl]-azetidine-1-carboxylic acid ethyl ester (50 mg, 0.11 mmol) was added 4 ml 2N NaOH/EtOH. The mixture was heated for 1 hour in a microwave. After cooling to room temperature 50% brine was added and the mixture extracted with dichloromethane. The combined organic layers were washed with brine, dried over sodium bicarbonate, filtered and the solvent evaporated. The residue was purified on 4 g SiO2 using 10% methanol in dichloromethane affording the desired product as a clear oil. m=15.5 mg
後処理
- temperatureThe mixture was heated for 1 hour in a microwave
- additionwas added
- extractionthe mixture extracted with dichloromethane
- washThe combined organic layers were washed with brine
- dry with materialdried over sodium bicarbonate
- filtrationfiltered
- customthe solvent evaporated
- customThe residue was purified on 4 g SiO2 using 10% methanol in dichloromethane affording the desired product as a clear oil
出典と根拠
- ORDレコード
- ord-b45ddf19bd5e48ad84259f297dd38baa
- 出典データセット
- uspto-grants-2014_11
- 特許番号
- US08877794B2
関連ノート
読み込み中…