Methanol → Methyl 2-(3-(bromomethyl)-4-methoxyphenyl)acetate

HRID 1617231노트

반응식

HRID 1617231 반응식
S(Cl)(Cl)=O.[Br:5][CH2:6][C:7]1[CH:8]=[C:9]([CH2:15][C:16]([OH:18])=[O:17])[CH:10]=[CH:11][C:12]=1[O:13][CH3:14].[CH3:19]O>>[Br:5][CH2:6][C:7]1[CH:8]=[C:9]([CH2:15][C:16]([O:18][CH3:19])=[O:17])[CH:10]=[CH:11][C:12]=1[O:13][CH3:14]

참가 물질

4

반응물 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 671652482-(3-(Bromomethyl)-4-methoxyphenyl)acetic acid

생성물 1

HCID 68416244Methyl 2-(3-(bromomethyl)-4-methoxyphenyl)acetate

반응 조건

온도
0 °C

실험 절차

Thionyl chloride (1.359 ml) was added dropwise to a solution of the product from step (i) (4.02 g) in MeOH (50 mL), the resulting suspension was stirred at 0° C. for 10 min then warmed to rt for 18 h. The solvent was evaporated and the residue was diluted with EtOAc washed with sat. NaHCO3 and sat. brine. The organic phase was dried, filtered and evaporated. The crude product was purified by chromatography, to give the subtitle compound as a yellow oil, 1.47 g.

후처리

  1. temperaturethen warmed to rt for 18 h
  2. customThe solvent was evaporated
  3. additionthe residue was diluted with EtOAc
  4. washwashed with sat. NaHCO3 and sat. brine
  5. customThe organic phase was dried
  6. filtrationfiltered
  7. customevaporated
  8. customThe crude product was purified by chromatography

출처 및 근거

ORD 기록
ord-b727c3e88d9c4334a39c4944ede2b3d8
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08765939B2

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