Sodium sulfate decahydrate → 5-tert-Butyl-1H-pyrazole-3-carbaldehyde

HRID 507952노트

반응식

HRID 507952 반응식
[C:1]([C:5]1[CH:9]=[C:8]([C:10](OCC)=[O:11])[NH:7][N:6]=1)([CH3:4])([CH3:3])[CH3:2].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>[O-2].[O-2].[Mn+4].O1CCCC1>[C:1]([C:5]1[CH:9]=[C:8]([CH:10]=[O:11])[NH:7][N:6]=1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

6

반응물 3

HCID 62649Sodium sulfate decahydrateHCID 2743509Ethyl 3-tert-butyl-1H-pyrazole-5-carboxylateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 1784410825-tert-Butyl-1H-pyrazole-3-carbaldehyde수율 69%

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매HCID 8028Tetrahydrofuran용매2회

실험 절차

To a mixture of ethyl 3-tert-butyl-1H-pyrazole-5-carboxylate (4.00 g, 20.4 mmol) and tetrahydrofuran (50 mL) was added lithium aluminum hydride (800 mg, 21.1 mmol) by small portions under ice-cooling, and the mixture was stirred at the same temperature for 1 hr. Sodium sulfate decahydrate (7.6 g) was added to the reaction mixture, and the insoluble material was filtered off. The filtrate was concentrated and a mixture of the obtained residue, manganese dioxide (10 g, 115 mmol) and tetrahydrofuran (100 mL) was stirred at room temperature for 3 hr. The insoluble material was filtered off, and the filtrate was concentrated to give the title compound (2.13 g, yield 69%) as colorless crystals.

후처리

  1. temperaturecooling
  2. filtrationthe insoluble material was filtered off
  3. concentrationThe filtrate was concentrated
  4. stirringwas stirred at room temperature for 3 hr
  5. filtrationThe insoluble material was filtered off
  6. concentrationthe filtrate was concentrated

출처 및 근거

ORD 기록
ord-46c3e544f55a478fa8482a4d4cb1a7f8
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07786165B2

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