反応式
[OH-].[Na+].C[O:4][C:5](=[O:31])/[CH:6]=[CH:7]/[C:8]1[CH:9]=[C:10]2[C:27](=[CH:28][CH:29]=1)[O:26][C:13]1([CH2:18][CH2:17][N:16]([C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])[CH2:15][CH2:14]1)[CH2:12][C:11]2=[O:30]>O.CO>[C:22]([O:21][C:19]([N:16]1[CH2:17][CH2:18][C:13]2([CH2:12][C:11](=[O:30])[C:10]3[C:27](=[CH:28][CH:29]=[C:8](/[CH:7]=[CH:6]/[C:5]([OH:31])=[O:4])[CH:9]=3)[O:26]2)[CH2:14][CH2:15]1)=[O:20])([CH3:25])([CH3:23])[CH3:24]参加物
5
反応条件
- 温度
- 50 °C
実験手順
NaOH (160 mg, 4 mmol) in H2O (2 ml) was added to a suspension of (E)-3-{1′-tert-butoxycarbonyl-4-oxo-spiro[chromane-2,4′-piperidine]-6-yl}-acrylic acid methyl ester (462 mg, 1.15 mmol, Intermediate 1, Step B) in MeOH (6 ml). The mixture was stirred at 50° C. After 2 h, MeOH was evaporated and the pH of the aqueous phase was adjusted with 1 M HCl to a pH value of 5. The resulting suspension was extracted with DCM, the organic phase dried over Na2SO4 and concentrated to give (E)-3-{1′-tert-butoxycarbonyl-4-oxo-spiro[chromane-2,4′-piperidine]-6-yl}-acrylic acid (410 mg) as a white solid.
後処理
- customMeOH was evaporated
- extractionThe resulting suspension was extracted with DCM
- dry with materialthe organic phase dried over Na2SO4
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-2186a312a4f844b5a4d75fe8181f1d4b
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09115148B2
関連ノート
読み込み中…