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

HRID 626715ノート

反応式

HRID 626715 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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+].

後処理

  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

出典と根拠

ORDレコード
ord-65a04e4ba9564b2385d5f51508280b3c
出典データセット
uspto-grants-2016_04
特許番号
US09309240B2

反応ノート

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