Benzyl 2-benzyl-4-oxo-3,4-dihydropyridine-1(2H)-carboxylate → HCID 21970317, 화합물

HRID 1033297노트

반응식

HRID 1033297 반응식
[CH2:1]([CH:8]1[CH2:13][C:12](=[O:14])[CH:11]=[CH:10][N:9]1C(OCC1C=CC=CC=1)=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>CO.[Pd].[Ni]>[CH2:1]([C@@H:8]1[CH2:13][C@H:12]([OH:14])[CH2:11][CH2:10][NH:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 1

HCID 19035856Benzyl 2-benzyl-4-oxo-3,4-dihydropyridine-1(2H)-carboxylate

생성물 1

HCID 21970317HCID 21970317, 화합물

시약·촉매·용매 3

HCID 935Nickel촉매HCID 23938Palladium촉매HCID 887Methanol용매2회

실험 절차

150 g (0.467 mol) of 2-benzyl-N-benzyloxycarbonyl-2,3-dihydro-4-(1H)-pyridone in 1.5 l of methanol are hydrogenated with 7.5 g of Pd/C (10%) as catalyst, then 50 g of Raney nickel and a further 200 ml of methanol are added, and hydrogenation is left to go to completion. Filtration is followed by evaporation in a rotary evaporator, and the brownish oil is chromatographed on silica gel with methylene chloride/methanol/conc. ammonia (60:10:1). The title compound is obtained as a semi-crystalline mass which is used further without additional purification. Crystallisation of a sample from ether/hexane yielded white crystals of melting point 111°-112°. TLC: methylene chloride/methanol/conc. ammonia (40:10:1) Rf =0.55, FD-MS: M+ =191.

후처리

  1. waithydrogenation is left
  2. filtrationFiltration
  3. customis followed by evaporation in a rotary evaporator
  4. customthe brownish oil is chromatographed on silica gel with methylene chloride/methanol/conc

출처 및 근거

ORD 기록
ord-30a0f180bfa943739cca95ad5324e28f
출처 데이터셋
uspto-grants-1994_05
특허 번호
US05310743

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