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

HRID 12921노트

반응식

HRID 12921 반응식
C([O:3][C:4]([C:6]1[CH:7]=[N:8][N:9]([CH:12]2[CH2:15][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][CH2:15]2)[N:8]=[CH:7][C:6]=1[C:4]([OH:5])=[O:3]

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 58972820HCID 58972820, 화합물

생성물 1

HCID 589728585-chloro-1-cyclobutyl-1H-pyrazole-4-carboxylic acid수율 94%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

To a solution of 5-chloro-1-cyclobutyl-1H-pyrazole-4-carboxylic acid ethyl ester (182 mg, 0.79 mmol) in methanol (8 mL) and water (8 mL) was added LiOH (23 mg, 0.96 mmol). The reaction mixture was stirred at reflux for 4 hours 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 layer was evaporated in vacuo to give 5-chloro-1-cyclobutyl-1H-pyrazole-4-carboxylic acid (148 mg, 94%) which was used without further purification.

후처리

  1. temperatureat reflux for 4 hours
  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 layer was evaporated in vacuo

출처 및 근거

ORD 기록
ord-dd3268c8f97946cc86e36fdf228ddcd2
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728029B2

반응 노트

불러오는 중…