Lithium Hydroxide → 5-chloro-1-cyclopropyl-1H-pyrazole-4-carboxylic acid

HRID 12911노트

반응식

HRID 12911 반응식
C([O:3][C:4]([C:6]1[CH:7]=[N:8][N:9]([CH:12]2[CH2:14][CH2:13]2)[C:10]=1[Cl:11])=[O:5])C.[Li+].[OH-]>CO.O>[Cl:11][C:10]1[N:9]([CH:12]2[CH2:13][CH2:14]2)[N:8]=[CH:7][C:6]=1[C:4]([OH:5])=[O:3]

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 67020969HCID 67020969, 화합물

생성물 1

HCID 670209125-chloro-1-cyclopropyl-1H-pyrazole-4-carboxylic acid수율 94%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

To a solution of 5-Chloro-1-cyclopropyl-1H-pyrazole-4-carboxylic acid ethyl ester (296 mg, 1.38 mmol) in methanol (15 mL) and water (15 mL) was added LiOH (40 mg, 1.66 mmol). The reaction mixture was stirred at reflux overnight and then concentrated under reduced pressure to remove the methanol. The residue was diluted with water, acidified to pH=2 with concentrated HCl, and extracted with ethyl acetate. The organic extracts were evaporated in vacuo to give 5-chloro-1-cyclopropyl-1H-pyrazole-4-carboxylic acid (242 mg, 93%) which was used without further purification.

후처리

  1. temperatureat reflux overnight
  2. concentrationconcentrated under reduced pressure
  3. customto remove the methanol
  4. additionThe residue was diluted with water
  5. extractionextracted with ethyl acetate
  6. customThe organic extracts were evaporated in vacuo

출처 및 근거

ORD 기록
ord-7f6daa50c3f1427aafab853c24e7447e
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728029B2

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