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Hydrochloric Acid → 6-(4-Fluorophenyl)-N4-[3-fluoro-4-(1H-pyrrolo[2,3-b]pyridin-4-yloxy)phenyl]-pyrimidine-2,4-diamine

HRID 16445
노트
인쇄 미리보기

반응식

HRID 16445 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:6]=[CH:7][C:8]=1[O:9][C:10]1[CH:15]=[CH:14][N:13]=[C:12]2[NH:16][CH:17]=[CH:18][C:11]=12)[NH2:5].Cl[C:20]1[CH:25]=[C:24]([C:26]2[CH:31]=[CH:30][C:29]([F:32])=[CH:28][CH:27]=2)[N:23]=[C:22]([NH2:33])[N:21]=1.Cl.C(=O)([O-])[O-].[Na+].[Na+]>O.CN(C)C=O.C(OCC)(=O)C>[F:32][C:29]1[CH:28]=[CH:27][C:26]([C:24]2[N:23]=[C:22]([NH2:33])[N:21]=[C:20]([NH:5][C:4]3[CH:6]=[CH:7][C:8]([O:9][C:10]4[CH:15]=[CH:14][N:13]=[C:12]5[NH:16][CH:17]=[CH:18][C:11]=45)=[C:2]([F:1])[CH:3]=3)[CH:25]=2)=[CH:31][CH:30]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 112183534-Chloro-6-(4-fluorophenyl)pyrimidin-2-amineHCID 160379654-((1H-Pyrrolo[2,3-B]pyridin-4-YL)oxy)-3-fluoroaniline

생성물 1

HCID 587332456-(4-Fluorophenyl)-N4-[3-fluoro-4-(1H-pyrrolo[2,3-b]pyridin-4-yloxy)phenyl]-pyrimidine-2,4-diamine

시약·촉매·용매 3

HCID 6228
Dimethylformamide
촉매
HCID 962Water용매
HCID 8857Ethyl Acetate용매

실험 절차

36 mg (0.15 mmol) of 3-fluoro-4-(1H-pyrrolo[2,3-b]pyridin-4-yloxy)aniline (from example XIX) and 38.5 mg (0.15 mmol) of 4-chloro-6-(4-fluorophenyl)pyrimidine-2-amine (from example LIX) are suspended in 1.5 ml of water, and 0.1 ml of 2 molar hydrochloric acid is added. The mixture is heated under reflux overnight. Ethyl acetate and a few drops of dimethylformamide are then added. The mixture is made alkaline using saturated sodium carbonate solution, the organic phase is separated off and the solvent is removed under reduced pressure. The product is purified by preparative HPLC.

후처리

  1. temperatureThe mixture is heated
  2. temperatureunder reflux overnight
  3. customthe organic phase is separated off
  4. customthe solvent is removed under reduced pressure
  5. customThe product is purified by preparative HPLC

출처 및 근거

ORD 기록
ord-6a13486060884f89b5d33e9e22cce4c7
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07737153B2

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