Methanol → 2-(Aminosulfonylamino)pentanoic acid methyl ester
反応式
C([NH:11][S:12]([NH:15][CH:16]([CH2:20][CH2:21][CH3:22])[C:17]([OH:19])=[O:18])(=[O:14])=[O:13])(OCC1C=CC=CC=1)=O.[CH3:23]O>[Pd]>[CH3:23][O:19][C:17](=[O:18])[CH:16]([NH:15][S:12]([NH2:11])(=[O:14])=[O:13])[CH2:20][CH2:21][CH3:22]参加物
4
実験手順
A mixture of 2-(N-carbobenzyloxyaminosulfonyl)aminopentanoic acid (46.7 g), methanol (350 mL) and 10% palladium on carbon (3.0 g) was hydrogenated at 55 psi for about 2 hours. The catalyst was removed by filtration through CELITE®, the solvent was removed in vacuo and the residue was purified by column chromatography on silica eluting with 50% ethyl acetate/hexane to afford 25.6 g (90%) of 2-(aminosulfonylamino)pentanoic acid methyl ester (Formula V: R=CH3 ; R1 =propyl; R2 =H; R3 =H), m.p. 63°-64° C.
後処理
- customThe catalyst was removed by filtration through CELITE®
- customthe solvent was removed in vacuo
- customthe residue was purified by column chromatography on silica eluting with 50% ethyl acetate/hexane
出典と根拠
- ORDレコード
- ord-ff6a248b0c284366b26da0c5aff681d4
- 出典データセット
- uspto-grants-1998_05
- 特許番号
- US05750546
反応ノート
読み込み中…