Methanol → 4-Chloro-3-(1-cyano-1-methylethyl)benzoic acid

HRID 1800563노트

반응식

HRID 1800563 반응식
[Cl:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8]C)=[O:7])=[CH:4][C:3]=1[C:12]([C:15]#[N:16])([CH3:14])[CH3:13].[OH-].[Li+].CO.O>O1CCCC1>[Cl:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[C:12]([C:15]#[N:16])([CH3:14])[CH3:13]

참가 물질

6

반응물 4

HCID 887MethanolHCID 962WaterHCID 3939Lithium HydroxideHCID 67312069Benzoic acid, 4-chloro-3-(1-cyano-1-methylethyl)-, methyl ester

생성물 1

HCID 668104254-Chloro-3-(1-cyano-1-methylethyl)benzoic acid수율 99%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of methyl 4-chloro-3-(1-cyano-1-methylethyl)benzoate (8.0 g, 34 mmol) in tetrahydrofuran (30 mL) were added lithium hydroxide.monohydrate (2.13 g, 51 mmol), methanol (100 mL) and water (5 mL), and the mixture was stirred at room temperature for 4 hr. The solvent was evaporated under reduced pressure, and the residue was diluted with water (200 mL). 1N Hydrochloric acid was slowly added to the mixture to adjust the pH to 3. The precipitated white precipitate was collected by filtration, washed with water, and dried to give the title compound (7.4 g, 99%) as a white powder.

후처리

  1. customThe solvent was evaporated under reduced pressure
  2. additionthe residue was diluted with water (200 mL)
  3. addition1N Hydrochloric acid was slowly added to the mixture
  4. filtrationThe precipitated white precipitate was collected by filtration
  5. washwashed with water
  6. customdried

출처 및 근거

ORD 기록
ord-5d53e512af59468f95034d753d926691
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08344135B2

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