Hydrochloric Acid → N-[2-Amino-6-chloro-4-pyrimidinyl]-N-[3-fluoro-4-(1H-indazol-5-yloxy)phenyl]amine

HRID 16437

반응식

HRID 16437 반응식
[NH2:1][C:2]1[CH:17]=[CH:16][C:5]([O:6][C:7]2[CH:8]=[C:9]3[C:13](=[CH:14][CH:15]=2)[NH:12][N:11]=[CH:10]3)=[C:4]([F:18])[CH:3]=1.[Cl:19][C:20]1[CH:25]=[C:24](Cl)[N:23]=[C:22]([NH2:27])[N:21]=1.Cl.C(=O)(O)[O-].[Na+]>O>[NH2:27][C:22]1[N:23]=[C:24]([NH:1][C:2]2[CH:17]=[CH:16][C:5]([O:6][C:7]3[CH:8]=[C:9]4[C:13](=[CH:14][CH:15]=3)[NH:12][N:11]=[CH:10]4)=[C:4]([F:18])[CH:3]=2)[CH:25]=[C:20]([Cl:19])[N:21]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 655222-Amino-4,6-dichloropyrimidineHCID 516892Sodium BicarbonateHCID 179792715-(4-Amino-2-fluorophenoxy)-1H-indazole

생성물 1

HCID 17979350N-[2-Amino-6-chloro-4-pyrimidinyl]-N-[3-fluoro-4-(1H-indazol-5-yloxy)phenyl]amine

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

1.65 g (6.78 mmol) of 5-(4-amino-2-fluorophenoxy)-1H-indazole (from example XII) are suspended in 90 ml of water. 1.11 g (6.78 mmol) of 4,6-dichloro-2-pyrimidineamine and 0.68 ml of concentrated aqueous hydrogen chloride solution are added, and the mixture is stirred at 100° C. overnight. For work-up, the reaction solution is made alkaline with saturated sodium bicarbonate solution and extracted 3× with ethyl acetate. The organic phase is dried with sodium sulfate and concentrated using a rotary evaporator.

후처리

  1. extractionextracted 3× with ethyl acetate
  2. dry with materialThe organic phase is dried with sodium sulfate
  3. concentrationconcentrated
  4. customa rotary evaporator

출처 및 근거

ORD 기록
ord-f49be5af1312475ea5319a61adc24c3e
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07737153B2

연결된 노트

불러오는 중…