Trifluoroacetic acid → HCID 11957741, 화합물

HRID 655942노트

반응식

HRID 655942 반응식
[Cl:1][C:2]1[C:3]([CH:9]2[CH2:11][CH:10]2[N:12]([C:20]([C:22]2[C:23]([CH:28]([F:30])[F:29])=[N:24][N:25]([CH3:27])[CH:26]=2)=[O:21])C(=O)OC(C)(C)C)=[N:4][CH:5]=[C:6]([Cl:8])[CH:7]=1.FC(F)(F)C(O)=O>ClCCl>[Cl:1][C:2]1[C:3]([CH:9]2[CH2:11][CH:10]2[NH:12][C:20]([C:22]2[C:23]([CH:28]([F:30])[F:29])=[N:24][N:25]([CH3:27])[CH:26]=2)=[O:21])=[N:4][CH:5]=[C:6]([Cl:8])[CH:7]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 66918177HCID 66918177, 화합물

생성물 1

HCID 11957741HCID 11957741, 화합물수율 85.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

0.200 g of tert-butyl [2-(3,5-dichloropyridin-2-yl)cyclopropyl]{[3-(difluoromethyl)-1-methyl-1H-pyrazol-4-yl]carbonyl}carbamate (0.00039 mol) are dissolved in 5 ml of dichloromethane. 0.50 ml of trifluoroacetic acid are added to the reaction mixture which is left stirring at room temperature overnight. The reaction mixture is quenched with 15 ml of an aqueous solution of saturated sodium bicarbonate. After separation, the aqueous phase is extracted with dichloromethane (10 ml). The combined organic phases are dried over magnesium sulfate, filtered, concentrated to dryness and purified on silica to yield to 120 mg of N-[2-(3,5-dichloropyridin-2-yl)cyclopropyl]-3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxamide (76%).

후처리

  1. waitis left
  2. customThe reaction mixture is quenched with 15 ml of an aqueous solution of saturated sodium bicarbonate
  3. customAfter separation
  4. extractionthe aqueous phase is extracted with dichloromethane (10 ml)
  5. dry with materialThe combined organic phases are dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated to dryness
  8. custompurified on silica

출처 및 근거

ORD 기록
ord-9dc09ef4331b4d809ec72c88cabcdfeb
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08071629B2

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