HCID 10014501、化合物 → 3-(Hydroxymethyl)-3,4-dihydroquinoxalin-2(1H)-one
反応式
C[O:2][C:3](=O)[CH:4]([CH2:15][OH:16])[NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[N+:12]([O-])=O>[Pd].CO>[OH:2][CH2:3][CH:4]1[NH:5][C:6]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[NH:12][C:15]1=[O:16]参加物
4
実験手順
A mixture of N-(2-nitrophenyl)-DL-serine methyl ester (XI, EXAMPLE 286, 0.506 g, 4.30 g), palladium on carbon (10%, 506 g) and 150 ml of methanol is shaken under hydrogen at 40 psi for 3.5 hr. The catalyst is then removed by filtration and the filtrate is concentrated under reduced pressure. The residue is then chromatographed on silica gel (400 ml) using eluting with methanol/methylene chloride (6/94), the appropriate fractions are pooled and concentrated to give the title compound, NMR (CDCl3) 2.70, 3.90, 4.00-4.18, 6.75, 6.92, 8.23. δ.
後処理
- customThe catalyst is then removed by filtration
- concentrationthe filtrate is concentrated under reduced pressure
- customThe residue is then chromatographed on silica gel (400 ml)
- washusing eluting with methanol/methylene chloride (6/94)
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-28833d30657348578d34a8550cb670e9
- 出典データセット
- uspto-grants-1996_07
- 特許番号
- US05541324
反応ノート
読み込み中…