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

HRID 1799260ノート

反応式

HRID 1799260 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-2c4307d252044f68be259e76ad5f2114
出典データセット
uspto-grants-2013_01
特許番号
US08344029B2

反応ノート

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