Lithium Hydroxide → HCID 67020984, 화합물

HRID 12912노트

반응식

HRID 12912 반응식
C([O:3][C:4]([C:6]1[CH:7]=[N:8][N:9]([CH2:15][CH:16]2[CH2:18][CH2:17]2)[C:10]=1[C:11]([F:14])([F:13])[F:12])=[O:5])C.[Li+].[OH-]>CO.O>[CH:16]1([CH2:15][N:9]2[C:10]([C:11]([F:12])([F:13])[F:14])=[C:6]([C:4]([OH:5])=[O:3])[CH:7]=[N:8]2)[CH2:18][CH2:17]1

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 670209131-cyclopropylmethyl-5-trifluoromethyl-1H-pyrazole-4-carboxylic acid ethyl ester

생성물 1

HCID 67020984HCID 67020984, 화합물수율 93%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

To a solution of 1-cyclopropylmethyl-5-trifluoromethyl-1H-pyrazole-4-carboxylic acid ethyl ester (120 mg, 0.46 mmol) in methanol (5 mL) and water (5 mL) was added LiOH (13 mg, 0.54 mmol). The reaction mixture was stirred at reflux overnight, and then the solution was concentrated under reduced pressure to remove the methanol. The residue was diluted with water and the solution was acidified to pH=2 with concentrated HCL. The resulting mixture was then extracted with ethyl acetate three times. The combined organic layers were concentrated in vacuo to give 1-cyclopropylmethyl-5-trifluoromethyl-1H-pyrazole-4-carboxylic acid (100 mg, 93%), which was used without further purification.

후처리

  1. temperatureat reflux overnight
  2. concentrationthe solution was concentrated under reduced pressure
  3. customto remove the methanol
  4. additionThe residue was diluted with water
  5. extractionThe resulting mixture was then extracted with ethyl acetate three times
  6. concentrationThe combined organic layers were concentrated in vacuo

출처 및 근거

ORD 기록
ord-b7f5194d744d48d4a0c4411e09c0c4d1
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728029B2

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