Lithium Hydroxide → 4-((2,2-Difluorocyclopropyl)methoxy)benzoic acid

HRID 1799260노트

반응식

HRID 1799260 반응식
[F:1][C:2]1([F:17])[CH2:4][CH:3]1[CH2:5][O:6][C:7]1[CH:16]=[CH:15][C:10]([C:11]([O:13]C)=[O:12])=[CH:9][CH:8]=1.[OH-].[Li+]>C(O)C>[F:1][C:2]1([F:17])[CH2:4][CH:3]1[CH2:5][O:6][C:7]1[CH:16]=[CH:15][C:10]([C:11]([OH:13])=[O:12])=[CH:9][CH:8]=1

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 69020821Methyl 4-[(2,2-difluorocyclopropyl)methoxy]benzoate

생성물 1

HCID 690200884-((2,2-Difluorocyclopropyl)methoxy)benzoic acid수율 95%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Methyl 4-[(2,2-difluorocyclopropyl)methoxy]benzoate (1.94 g, 8.01 mmol) prepared in Example 40 (40a) was dissolved in ethanol (24 mL), and a 2 M lithium hydroxide aqueous solution (8 mL, 16 mmol) was added thereto at room temperature. The resulting mixture was stirred at the same temperature for 18 hours. The solvents (mainly ethanol) were evaporated, and water was added to the obtained residue. Then, the resulting mixture was changed to weak acidic by adding 2 N hydrochloric acid under ice-cooling with stirring. The precipitated insoluble substance was collected by filtration, washed with water and n-hexane, and dried under reduced pressure to give 1.73 g of the title compound (white powder, yield: 95%).

후처리

  1. customat room temperature
  2. customThe solvents (mainly ethanol) were evaporated
  3. additionwater was added to the obtained residue
  4. additionby adding 2 N hydrochloric acid under ice-
  5. temperaturecooling
  6. stirringwith stirring
  7. filtrationThe precipitated insoluble substance was collected by filtration
  8. washwashed with water and n-hexane
  9. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-2c4307d252044f68be259e76ad5f2114
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08344029B2

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