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

HRID 505512노트

반응식

HRID 505512 반응식
[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

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 178509921HCID 178509921, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 6212Chloroform용매

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-d8e444afc0434e4cbd2a45d269e7c9ab
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07781454B2

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