N-(4-Methoxyphenyl)-4-(pyridin-3-yl)pyrimidin-2-amine → 4-[[4-(3-Pyridinyl)-2-pyrimidinyl]amino]phenol

HRID 2352177노트

반응식

HRID 2352177 반응식
C[O:2][C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10]2[N:15]=[C:14]([C:16]3[CH:17]=[N:18][CH:19]=[CH:20][CH:21]=3)[CH:13]=[CH:12][N:11]=2)=[CH:5][CH:4]=1>Br>[N:18]1[CH:19]=[CH:20][CH:21]=[C:16]([C:14]2[CH:13]=[CH:12][N:11]=[C:10]([NH:9][C:6]3[CH:7]=[CH:8][C:3]([OH:2])=[CH:4][CH:5]=3)[N:15]=2)[CH:17]=1

참가 물질

3

반응물 1

HCID 14346975N-(4-Methoxyphenyl)-4-(pyridin-3-yl)pyrimidin-2-amine

생성물 1

HCID 143471904-[[4-(3-Pyridinyl)-2-pyrimidinyl]amino]phenol

시약·촉매·용매 1

HCID 260Hydrogen Bromide용매

실험 절차

A 25.0 g portion of N-(4-methoxyphenyl)-4-(3-pyridinyl)-2-pyrimidinamine was dissolved in 200 ml of 48% hydrobromic acid and stirred overnight under an argon atmosphere. The mixture was then heated on a steam bath for 7 hours, cooled overnight and evaporated at 60° C. The residue was basified with 200 ml of saturated potassium bicarbonate solution and stirred for 1.5 hours. The solid was collected, washed with water, dried and recrystallized from hot absolute ethanol, giving 19.1 g of the desired product, mp 223°-225° C.

후처리

  1. temperatureThe mixture was then heated on a steam bath for 7 hours
  2. temperaturecooled overnight
  3. customevaporated at 60° C
  4. stirringstirred for 1.5 hours
  5. customThe solid was collected
  6. washwashed with water
  7. customdried
  8. customrecrystallized from hot absolute ethanol

출처 및 근거

ORD 기록
ord-83ccaa319ea244c4a4dc7de81e4c1931
출처 데이터셋
uspto-grants-1989_10
특허 번호
US04876252

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