Hydrochloric Acid → 3-[1-[(6-amino-2H-pyrazolo[3,4-b]pyridin-3-yl)methyl]-5-chloroindazol-4-yl]oxy-5-chlorobenzonitrile;hydrochloride

HRID 505512ノート

反応式

HRID 505512 の反応式
[NH2:1][C:2]1[N:7]=[C:6]2[NH:8][N:9]=[C:10]([CH2:11][N:12]3[C:20]4[C:15](=[C:16]([O:22][C:23]5[CH:24]=[C:25]([CH:28]=[C:29]([Cl:31])[CH:30]=5)[C:26]#[N:27])[C:17]([Cl:21])=[CH:18][CH:19]=4)[CH:14]=[N:13]3)[C:5]2=[CH:4][CH:3]=1.Cl>CO.C(Cl)(Cl)Cl>[Cl-:21].[Cl:21][C:17]1[C:16]([O:22][C:23]2[CH:24]=[C:25]([C:26]#[N:27])[CH:28]=[C:29]([Cl:31])[CH:30]=2)=[C:15]2[C:20](=[CH:19][CH:18]=1)[N:12]([CH2:11][C:10]1[C:5]3[C:6](=[N:7][C:2]([NH3+:1])=[CH:3][CH:4]=3)[NH:8][N:9]=1)[N:13]=[CH:14]2

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 178509921HCID 178509921、化合物

生成物 1

HCID 1785099223-[1-[(6-amino-2H-pyrazolo[3,4-b]pyridin-3-yl)methyl]-5-chloroindazol-4-yl]oxy-5-chlorobenzonitrile;hydrochloride

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6212Chloroform溶媒

実験手順

To 3-({1-[(6-amino-1H-pyrazolo[3,4-b]pyridin-3-yl)methyl]-5-chloro-1H-indazol-4-yl}oxy)-5-chlorobenzonitrile (0.936 g, 2.079 mmol) as a solution in 20% methanol in chloroform (300 mL) was added 1N HCl (2.079 mL, 2.079 mmol), and the resulting mixture was then concentrated under reduced pressure. The resulting white paste was diluted with acetonitrile (100 mL) and the solvent evaporated in vacuo. The dilution-evaporation was repeated twice more for a total of three times. The resulting residue was placed under vacuum overnight to give product. 1H NMR (DMSO-d6): 6.7.91 (s, 1H), 7.81 (s, 3H), 7.68-7.60 (m, 2H), 7.48 (s, 1H), 7.37 (s, 1H), 6.50-6.30 (m, 2H), 6.00-5.86 (m, 2H). HRMS (M+1)=450.06

後処理

  1. concentrationthe resulting mixture was then concentrated under reduced pressure
  2. additionThe resulting white paste was diluted with acetonitrile (100 mL)
  3. customthe solvent evaporated in vacuo
  4. customThe dilution-evaporation
  5. customwas placed under vacuum overnight
  6. customto give product

出典と根拠

ORDレコード
ord-d8e444afc0434e4cbd2a45d269e7c9ab
出典データセット
uspto-grants-2010_08
特許番号
US07781454B2

反応ノート

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