HCID 10014501, 화합물 → 3-(Hydroxymethyl)-3,4-dihydroquinoxalin-2(1H)-one
반응식
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]참가 물질
4
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-28833d30657348578d34a8550cb670e9
- 출처 데이터셋
- uspto-grants-1996_07
- 특허 번호
- US05541324
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