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

HRID 2352177ノート

反応式

HRID 2352177 の反応式
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

参加物

3

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 260Hydrogen Bromide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-83ccaa319ea244c4a4dc7de81e4c1931
出典データセット
uspto-grants-1989_10
特許番号
US04876252

反応ノート

読み込み中…