Methanol → 2-Chloro-3-(1-cyano-1-methylethyl)benzoic acid

HRID 1800702노트

반응식

HRID 1800702 반응식
[Cl:1][C:2]1[C:11]([C:12]([C:15]#[N:16])([CH3:14])[CH3:13])=[CH:10][CH:9]=[CH:8][C:3]=1[C:4]([O:6]C)=[O:5].CO.O.O.[OH-].[Li+]>O1CCCC1>[Cl:1][C:2]1[C:11]([C:12]([C:15]#[N:16])([CH3:14])[CH3:13])=[CH:10][CH:9]=[CH:8][C:3]=1[C:4]([OH:6])=[O:5]

참가 물질

6

반응물 4

HCID 887MethanolHCID 962WaterHCID 168937Lithium hydroxide, monohydrateHCID 67312408Methyl 2-chloro-3-(1-cyano-1-methylethyl)benzoate

생성물 1

HCID 668102752-Chloro-3-(1-cyano-1-methylethyl)benzoic acid수율 91.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of methyl 2-chloro-3-(1-cyano-1-methylethyl)benzoate (1.67 g, 7.02 mmol) in tetrahydrofuran (24 mL)/methanol (8 mL)/water (8 mL) was added lithium hydroxide-monohydrate (501 mg, 11.9 mmol), and the mixture was stirred at room temperature for 2 hr. The reaction mixture was concentrated under reduced pressure, and 6N hydrochloric acid (2.8 mL) was added dropwise to the residue. The precipitate was collected by filtration, and washed with water to give the title compound (1.43 g, 91%) as a white powder.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure, and 6N hydrochloric acid (2.8 mL)
  2. additionwas added dropwise to the residue
  3. filtrationThe precipitate was collected by filtration
  4. washwashed with water

출처 및 근거

ORD 기록
ord-30f7642a9cc24c6487e1255607344a51
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08344135B2

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