6-[1-Hydroxy-2-methyl-1-(1-trityl-1H-imidazol-4-yl)propyl]naphthalen-2-yloxymethyl 2,2-dimethylpropionate → HCID 178450085, 화합물

HRID 1368535

반응식

HRID 1368535 반응식
[CH3:1][C:2]([CH3:48])([CH3:47])[C:3]([O:5][CH2:6][O:7][C:8]1[CH:17]=[CH:16][C:15]2[C:10](=[CH:11][CH:12]=[C:13]([C:18]([OH:46])([C:22]3[N:23]=[CH:24][N:25](C(C4C=CC=CC=4)(C4C=CC=CC=4)C4C=CC=CC=4)[CH:26]=3)[CH:19]([CH3:21])[CH3:20])[CH:14]=2)[CH:9]=1)=[O:4]>C(O)(=O)C.[C].[Pd]>[CH3:48][C:2]([CH3:1])([CH3:47])[C:3]([O:5][CH2:6][O:7][C:8]1[CH:17]=[CH:16][C:15]2[C:10](=[CH:11][CH:12]=[C:13]([C:18]([OH:46])([C:22]3[N:23]=[CH:24][NH:25][CH:26]=3)[CH:19]([CH3:21])[CH3:20])[CH:14]=2)[CH:9]=1)=[O:4]

참가 물질

4

반응물 1

HCID 220184286-[1-Hydroxy-2-methyl-1-(1-trityl-1H-imidazol-4-yl)propyl]naphthalen-2-yloxymethyl 2,2-dimethylpropionate

생성물 1

HCID 178450085HCID 178450085, 화합물수율 45.2%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 176Acetic Acid용매

반응 조건

온도
50 °C

실험 절차

6-[1-Hydroxy-2-methyl-1-(1-trityl-1H-imidazol-4-yl)propyl]naphthalen-2-yloxymethyl 2,2-dimethylpropionate (0.381 g) was dissolved in acetic acid (15 ml). To the solution was added palladium carbon (0.200 g), and the mixture was stirred at 50° C. for 2 h under hydrogen atmosphere. The catalyst was filtered off, and the filtrate was concentrated under reduced pressure. To the residue was added ethyl acetate, and the mixture was washed with saturated aqueous solution of sodium hydrogencarbonate and saturated sodium chloride solution. The organic layer was dried and concentrated. The obtained residue was purified by silica gel column chromatography (eluent, dichloromethane:methanol=30:1→20:1) to give the titled compound (0.107 g) as an amorphous product.

후처리

  1. filtrationThe catalyst was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. additionTo the residue was added ethyl acetate
  4. washthe mixture was washed with saturated aqueous solution of sodium hydrogencarbonate and saturated sodium chloride solution
  5. customThe organic layer was dried
  6. concentrationconcentrated
  7. customThe obtained residue was purified by silica gel column chromatography (eluent, dichloromethane:methanol=30:1→20:1)

출처 및 근거

ORD 기록
ord-4854da9b5a3d4bdf8d422a7bafbba0c4
출처 데이터셋
uspto-grants-2003_06
특허 번호
US06573289B1

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