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Lithium Hydroxide → 5-Bromo-2-[(4-fluorobenzyl)oxy]benzoic acid

HRID 1623709
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인쇄 미리보기

반응식

HRID 1623709 반응식
[OH-].[Li+].[Br:3][C:4]1[CH:5]=[CH:6][C:7]([O:21][CH2:22][C:23]2[CH:28]=[CH:27][C:26]([F:29])=[CH:25][CH:24]=2)=[C:8]([CH:20]=1)[C:9]([O:11]CC1C=CC(F)=CC=1)=[O:10]>O.O1CCCC1>[Br:3][C:4]1[CH:5]=[CH:6][C:7]([O:21][CH2:22][C:23]2[CH:24]=[CH:25][C:26]([F:29])=[CH:27][CH:28]=2)=[C:8]([CH:20]=1)[C:9]([OH:11])=[O:10]
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참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 67107744(4-Fluorophenyl)methyl 5-bromo-2-{[(4-fluorophenyl)methyl]oxy}benzoate

생성물 1

HCID 87068895-Bromo-2-[(4-fluorobenzyl)oxy]benzoic acid

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

Lithium hydroxide (0.43 g, 18.14 mmol) was added to a solution of (4-fluorophenyl)methyl 5-bromo-2-{[(4-fluorophenyl)methyl]oxy}benzoate (may be prepared as described in Description 86) (2.62 g, 6.05 mmol) in water (5 ml) and tetrahydrofuran (20 ml). The mixture was stirred overnight and the solvent removed in vacuo. The residue was redissolved in water (30 ml) and acidified to pH=2 using 1N HCl and then extracted with ethyl acetate (3×25 ml). The combined organic layers were dried (MgSO4) and the solvent removed in vacuo to yield the titled compound as a white solid. 1.97 g.

후처리

  1. customthe solvent removed in vacuo
  2. dissolutionThe residue was redissolved in water (30 ml)
  3. extractionextracted with ethyl acetate (3×25 ml)
  4. dry with materialThe combined organic layers were dried (MgSO4)
  5. customthe solvent removed in vacuo

출처 및 근거

ORD 기록
ord-4097d200e93741f183d0e7440778c941
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08778939B2

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