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2-(3-Bromo-4-fluoro-alpha-hydroxybenzyl)-3-methoxymethoxypyridine → 2-(3-Bromo-4-fluorobenzoyl)-3-methoxymethoxypyridine

HRID 442722
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반응식

HRID 442722 반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH:17]=[CH:18][C:19]=1[F:20])[CH:5]([C:7]1[C:12]([O:13][CH2:14][O:15][CH3:16])=[CH:11][CH:10]=[CH:9][N:8]=1)[OH:6]>[O-2].[O-2].[Mn+4].C(OCC)(=O)C>[Br:1][C:2]1[CH:3]=[C:4]([CH:17]=[CH:18][C:19]=1[F:20])[C:5]([C:7]1[C:12]([O:13][CH2:14][O:15][CH3:16])=[CH:11][CH:10]=[CH:9][N:8]=1)=[O:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 539404062-(3-Bromo-4-fluoro-alpha-hydroxybenzyl)-3-methoxymethoxypyridine

생성물 1

HCID 539864842-(3-Bromo-4-fluorobenzoyl)-3-methoxymethoxypyridine수율 93.4%

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 2-(3-bromo-4-fluoro-α-hydroxy-benzyl)-3-methoxymethoxypyridine (14.0 g), activated manganese dioxide (41.8 g) and ethyl acetate (200 mL) was stirred overnight at room temperature, which was then subjected to filtration. The filtrate was concentrated under reduced pressure. The concentrate was purified by means of a silica gel column (ethyl acetate--hexane) to afford 2-(3-bromo-4-fluorobenzoyl)-3-methoxymethoxypyridine (13.0 g) (compound B-5). Physical properties and spectrum data of the product are shown in Table 3 and Table 4.

후처리

  1. filtrationwhich was then subjected to filtration
  2. concentrationThe filtrate was concentrated under reduced pressure
  3. customThe concentrate was purified by means of a silica gel column (ethyl acetate--hexane)

출처 및 근거

ORD 기록
ord-7b1ea55e66054eb0abdeaf0b8c370e45
출처 데이터셋
uspto-grants-1999_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05891895

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