Methanol → Methyl 2-(5-bromopyridin-3-yl)acetate

HRID 445767

반응식

HRID 445767 반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH2:8][C:9]([OH:11])=[O:10])[CH:5]=[N:6][CH:7]=1.S(=O)(=O)(O)O.[CH3:17]O>>[CH3:17][O:10][C:9](=[O:11])[CH2:8][C:4]1[CH:5]=[N:6][CH:7]=[C:2]([Br:1])[CH:3]=1

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 28025392-(5-Bromopyridin-3-yl)acetic acid

생성물 1

HCID 23398394Methyl 2-(5-bromopyridin-3-yl)acetate

실험 절차

A mixture of (5-bromo-pyridin-3-yl)-acetic acid (ABCR, Karlsruhe, Germany, 4.54 mmol) and concentrated sulfuric acid (0.02 ml) in MeOH was refluxed for 13.5 h. The RM was concentrated, taken in EtOAc and sonicated. The organic layer was washed with saturated aqueous NaHCO3, with brine, dried over Na2SO4, filtered and evaporated to dryness to give the title compound as a brown oil. (HPLC: tR 2.21 min (Method A); M+H=230, 232 MS-ES)

후처리

  1. temperaturewas refluxed for 13.5 h
  2. concentrationThe RM was concentrated
  3. customsonicated
  4. washThe organic layer was washed with saturated aqueous NaHCO3, with brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. customevaporated to dryness

출처 및 근거

ORD 기록
ord-f336233cdd9e4e0db0c80e3722d06f41
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08476294B2

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