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Sodium sulfate decahydrate → [4-(Diphenylmethoxy)-3-isobutylphenyl]methanol

HRID 507994
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HRID 507994 반응식
[C:1]1([CH:7]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[O:8][C:9]2[CH:18]=[CH:17][C:12]([C:13](OC)=[O:14])=[CH:11][C:10]=2[CH2:19][CH:20]([CH3:22])[CH3:21])[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([CH:7]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[O:8][C:9]2[CH:18]=[CH:17][C:12]([CH2:13][OH:14])=[CH:11][C:10]=2[CH2:19][CH:20]([CH3:22])[CH3:21])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 23157404Methyl 4-(diphenylmethoxy)-3-isobutylbenzoate

생성물 1

HCID 23157345[4-(Diphenylmethoxy)-3-isobutylphenyl]methanol수율 101%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of methyl 4-(diphenylmethoxy)-3-isobutylbenzoate (0.45 g, 1.20 mmol) in tetrahydrofuran (20 mL) was added lithium aluminum hydride (60 mg, 1.58 mmol) by small portions under ice-cooling. The mixture was stirred under ice-cooling for 2 hr, sodium sulfate decahydrate (1.2 g, 2.30 mmol) was added to the reaction solution by small portions, and the mixture was stirred at room temperature for 1 hr. The insoluble material was filtered off, and the filtrate was concentrated to give the title compound (420 mg, yield 100%) as a colorless oil.

후처리

  1. temperaturecooling
  2. temperaturecooling for 2 hr
  3. stirringthe mixture was stirred at room temperature for 1 hr
  4. filtrationThe insoluble material was filtered off
  5. concentrationthe filtrate was concentrated

출처 및 근거

ORD 기록
ord-f94b99147b0442d09b3231b7d7c71642
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07786165B2

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