Ammonium Hydroxide → N-(2-amino-6-chloro-4-pyrimidinyl)-N-[3-fluoro-4-(4-pyridinylsulfanyl)phenyl]amine

HRID 496019노트

반응식

HRID 496019 반응식
[NH2:1][C:2]1[N:7]=[C:6]([Cl:8])[CH:5]=[C:4](Cl)[N:3]=1.[F:10][C:11]1[CH:12]=[C:13]([CH:15]=[CH:16][C:17]=1[S:18][C:19]1[CH:24]=[CH:23][N:22]=[CH:21][CH:20]=1)[NH2:14].[OH-].[NH4+]>O.Cl>[NH2:1][C:2]1[N:3]=[C:4]([NH:14][C:13]2[CH:15]=[CH:16][C:17]([S:18][C:19]3[CH:24]=[CH:23][N:22]=[CH:21][CH:20]=3)=[C:11]([F:10])[CH:12]=2)[CH:5]=[C:6]([Cl:8])[N:7]=1

참가 물질

6

반응물 3

HCID 14923Ammonium HydroxideHCID 655222-Amino-4,6-dichloropyrimidineHCID 70592743-Fluoro-4-(4-pyridinylsulfanyl)aniline

생성물 1

HCID 22324284N-(2-amino-6-chloro-4-pyrimidinyl)-N-[3-fluoro-4-(4-pyridinylsulfanyl)phenyl]amine수율 47.4%

시약·촉매·용매 2

HCID 313Hydrochloric Acid촉매HCID 962Water용매

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온도
100 °C

실험 절차

2-Amino-4,6 dichloropyrimidine (A21, 12 mmol) and 3-fluoro-4-(4-pyridinylthio)-aniline (B7,12 mmol) were suspended in water (150 mL) and treated with 10 drops of concentrated hydrochloric acid. The mixture was stirred at 100° C. overnight. The clear solution was then neutralized with ammonium hydroxide. The precipitated yellow product was filtered, washed with water, and purified by column chromatography with 1-3% MeOH in CH2Cl2 to give the desired product as a white solid (1.98 g, 47%).

후처리

  1. filtrationThe precipitated yellow product was filtered
  2. washwashed with water
  3. custompurified by column chromatography with 1-3% MeOH in CH2Cl2

출처 및 근거

ORD 기록
ord-75b5f6d320e5437e882924ed062ada56
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06943172B2

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