Trifluoroacetic acid → 7-Chloro-2-(2,6-dichlorophenyl)-2H-pyrazolo[4,3-c]pyridin-4-ylamine

HRID 626715노트

반응식

HRID 626715 반응식
C(OC(=O)[NH:7][C:8]1[C:13]2=[CH:14][N:15]([C:17]3[C:22]([Cl:23])=[CH:21][CH:20]=[CH:19][C:18]=3[Cl:24])[N:16]=[C:12]2[C:11]([Cl:25])=[CH:10][N:9]=1)(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl>[Cl:25][C:11]1[C:12]2[C:13](=[CH:14][N:15]([C:17]3[C:22]([Cl:23])=[CH:21][CH:20]=[CH:19][C:18]=3[Cl:24])[N:16]=2)[C:8]([NH2:7])=[N:9][CH:10]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 69671401[7-chloro-2-(2,6-dichlorophenyl)-2H-pyrazolo[4,3-c]pyridin-4-yl]-carbamic acid tert-butyl ester

생성물 1

HCID 696711997-Chloro-2-(2,6-dichlorophenyl)-2H-pyrazolo[4,3-c]pyridin-4-ylamine수율 24,845.199%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of [7-chloro-2-(2,6-dichlorophenyl)-2H-pyrazolo[4,3-c]pyridin-4-yl]-carbamic acid tert-butyl ester (531 mg, contaminated with residual tert-butyl carbamate) and TFA (10 mL) in DCM (10 mL) was stirred at room temperature for 2 h and then concentrated under reduced pressure. The residue was partitioned between ethyl acetate and sodium bicarbonate (sat. aq.). The organic layer was washed with brine, dried over anhydrous sodium sulfate, and concentrated to dryness under reduced pressure to afford the title compound as a beige solid (100 g, 30% yield over 2 steps). LCMS (Method D): RT=2.15 min, m/z: 313 [M+H+].

후처리

  1. concentrationconcentrated under reduced pressure
  2. customThe residue was partitioned between ethyl acetate and sodium bicarbonate (sat. aq.)
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated to dryness under reduced pressure

출처 및 근거

ORD 기록
ord-65a04e4ba9564b2385d5f51508280b3c
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09309240B2

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