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Hexane → HCID 69423063, 화합물

HRID 349985
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HRID 349985 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([O:14][C:15]1[CH:38]=[CH:37][C:18]([CH2:19][N:20]2[CH:24]=[C:23]([C:25](OCC)=[O:26])[C:22]([C:30]3[CH:35]=[CH:34][C:33]([F:36])=[CH:32][CH:31]=3)=[N:21]2)=[CH:17][CH:16]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+].CCCCCC>O1CCCC1>[CH2:7]([O:14][C:15]1[CH:38]=[CH:37][C:18]([CH2:19][N:20]2[CH:24]=[C:23]([CH2:25][OH:26])[C:22]([C:30]3[CH:31]=[CH:32][C:33]([F:36])=[CH:34][CH:35]=3)=[N:21]2)=[CH:17][CH:16]=1)[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8058HexaneHCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 23024738HCID 23024738, 화합물

생성물 1

HCID 69423063HCID 69423063, 화합물수율 95%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매

실험 절차

Lithium aluminium hydride (1.33 g) was added to a solution of ethyl 1-(4-benzyloxybenzyl)-3-(4-fluorophenyl)-1H-pyrazole-4-carboxylate (15.1 g) in tetrahydrofuran (300 ml) at 0° C., which was stirred at room temperature for 1 hour. Sodium sulfate decahydrate (12.26 g) and hexane (100 ml) was added to the reaction mixture, which was stirred at room temperature for 1 hour. After the precipitate was removed by filtration, the filtrate was concentrated to obtain 1-(4-benzyloxybenzyl)-3-(4-fluorophenyl)-1H-pyrazol-4-ylmethanol (12.9 g, yield 95%) as colorless crystals. This was recrystallized from ethyl acetate-hexane. Melting point: 112–113° C.

후처리

  1. stirringwas stirred at room temperature for 1 hour
  2. customAfter the precipitate was removed by filtration
  3. concentrationthe filtrate was concentrated

출처 및 근거

ORD 기록
ord-ddb74aa6cc80416d83a23c476903228a
출처 데이터셋
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07179823B1

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