Sodium sulfate decahydrate → HCID 23157461, 화합물

HRID 2110862노트

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HRID 2110862 반응식
[C:1]1([C:7]2[CH:11]=[C:10]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[N:9]([CH2:18][C:19]3[CH:28]=[CH:27][C:22]([C:23](OC)=[O:24])=[CH:21][C:20]=3[O:29][CH:30]([CH3:32])[CH3:31])[N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[C:1]1([C:7]2[CH:11]=[C:10]([C:12]3[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=3)[N:9]([CH2:18][C:19]3[CH:28]=[CH:27][C:22]([CH2:23][OH:24])=[CH:21][C:20]=3[O:29][CH:30]([CH3:32])[CH3:31])[N:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

5

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HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 23157367methyl 4-[(3,5-diphenyl-1H-pyrazol-1-yl)methyl]-3-isopropoxybenzoate

생성물 1

HCID 23157461HCID 23157461, 화합물수율 92%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

To a solution of methyl 4-[(3,5-diphenyl-1H-pyrazol-1-yl)methyl]-3-isopropoxybenzoate (0.59 g, 1.38 mmol) in tetrahydrofuran (12 mL) was added lithium aluminum hydride (52 mg, 1.38 mmol) with stirring at 0° C., and the mixture was stirred at the same temperature for 2.5 hr. After completion of the reaction, sodium sulfate decahydrate (0.89 g, 2.76 mmol) was added to the reaction mixture, and the mixture was stirred at room temperature for 2 hr. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=5/1-hexane/ethyl acetate=1/1) to give the title compound (0.50 g, yield 92%) as a colorless oil. MS (ESI+): 399 (M+H).

후처리

  1. stirringthe mixture was stirred at the same temperature for 2.5 hr
  2. additionwas added to the reaction mixture
  3. stirringthe mixture was stirred at room temperature for 2 hr
  4. filtrationThe insoluble material was filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=5/1-hexane/ethyl acetate=1/1)

출처 및 근거

ORD 기록
ord-e521ddfe5258452abea2008398da02aa
출처 데이터셋
uspto-grants-2009_04
특허 번호
US07517910B2

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