Dichloromethane → HCID 71138925、化合物

HRID 1914016ノート

反応式

HRID 1914016 の反応式
[NH2:1][C:2]1[C:7]([C:8]2[N:31]([C:32]3[CH:37]=[CH:36][C:35]([C:38]4([NH:42]C(=O)OC(C)(C)C)[CH2:41][CH2:40][CH2:39]4)=[CH:34][CH:33]=3)[C:11]3=[N:12][C:13]([C:16]4[CH:21]=[CH:20][CH:19]=[C:18]([NH:22][C:23]([CH:25]5[CH2:30][CH2:29][O:28][CH2:27][CH2:26]5)=[O:24])[CH:17]=4)=[CH:14][CH:15]=[C:10]3[N:9]=2)=[CH:6][CH:5]=[CH:4][N:3]=1.FC(F)(F)C(O)=O.[Cl:57]CCl>>[ClH:57].[NH2:42][C:38]1([C:35]2[CH:34]=[CH:33][C:32]([N:31]3[C:11]4=[N:12][C:13]([C:16]5[CH:17]=[C:18]([NH:22][C:23]([CH:25]6[CH2:30][CH2:29][O:28][CH2:27][CH2:26]6)=[O:24])[CH:19]=[CH:20][CH:21]=5)=[CH:14][CH:15]=[C:10]4[N:9]=[C:8]3[C:7]3[C:2]([NH2:1])=[N:3][CH:4]=[CH:5][CH:6]=3)=[CH:37][CH:36]=2)[CH2:39][CH2:40][CH2:41]1

参加物

4

反応物 3

HCID 6344DichloromethaneHCID 6422Trifluoroacetic acidHCID 71142507HCID 71142507、化合物

生成物 1

HCID 71138925HCID 71138925、化合物

実験手順

To a solution of tert-butyl (1-{4-[2-(2-aminopyridin-3-yl)-5-{3-[(tetrahydro-2H-pyran-4-ylcarbonyl)amino]phenyl}-3H-imidazo[4,5-b]pyridin-3-yl]phenyl}cyclobutyl)carbamate (29 mg) in dichloromethane (4 mL) was added trifluoroacetic acid (1 mL) dropwise at room temperature. After being stirred at the same temperature for 1 h, the reaction mixture was concentrated under reduced pressure. Dichloromethane (5 mL) and MP-carbonate (Argonaout technologies 2.91 mmol/g, 400 mg) were added. The mixture was stayed for 30 min. with occasional shaking then filtered. The filtrate was concentrated under reduced pressure. To a solution of the residue in dichloromethane (5 mL) and methanol (0.4 mL) was added hydrogen chloride in ethyl acetate (4 M, 0.055 mL) at room temperature. After being stirred for 10 min., the mixture was concentrated under reduced pressure. The resulting solid was suspended with ethyl acetate and filtered to give the product (19 mg).

後処理

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. additionDichloromethane (5 mL) and MP-carbonate (Argonaout technologies 2.91 mmol/g, 400 mg) were added
  3. waitThe mixture was stayed for 30 min.
  4. stirringwith occasional shaking
  5. filtrationthen filtered
  6. concentrationThe filtrate was concentrated under reduced pressure
  7. additionTo a solution of the residue in dichloromethane (5 mL) and methanol (0.4 mL) was added hydrogen chloride in ethyl acetate (4 M, 0.055 mL) at room temperature
  8. stirringAfter being stirred for 10 min.
  9. concentrationthe mixture was concentrated under reduced pressure
  10. filtrationfiltered

出典と根拠

ORDレコード
ord-47e83fe8e3a24285920ab13117eadff9
出典データセット
uspto-grants-2013_12
特許番号
US08609688B2

反応ノート

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