Butylamine → 3-Butylamino-6-(2,6-dichlorophenyl)-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one

HRID 3186

反応式

HRID 3186 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:20](=[O:21])[N:19]([CH3:22])[C:12]2[N:13]=[C:14](SC)[N:15]=[CH:16][C:11]=2[CH:10]=1.[CH2:23]([NH2:27])[CH2:24][CH2:25][CH3:26]>CN(C)C=O>[CH2:23]([NH:27][N:15]1[CH:16]=[C:11]2[CH:10]=[C:9]([C:3]3[C:2]([Cl:1])=[CH:7][CH:6]=[CH:5][C:4]=3[Cl:8])[C:20](=[O:21])[N:19]([CH3:22])[C:12]2=[N:13][CH2:14]1)[CH2:24][CH2:25][CH3:26]

参加物

4

反応物 2

HCID 8007ButylamineHCID 107367016-(2,6-Dichlorophenyl)-8-methyl-2-(methylthio)pyrido[2,3-d]pyrimidin-7(8H)-one

生成物 1

HCID 867523433-Butylamino-6-(2,6-dichlorophenyl)-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
110 °C

実験手順

A mixture of 0.177 g (0.50 mmol) of 6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 37, 10 mL of n-butylamine and 1.0 mL of dimethylformamide was heated with stirring to reflux (110° C. oil bath). After 1 hour, solution was complete. After 20 hours reflux, the excess amine and dimethylformamide were evaporated, and the residue was triturated with water, filtered, washed with water, and dried; wt 0.180 g. Recrystallization from ethyl acetate/petroleum ether gave pure product; wt 0.116 g; mp 184°-186° C.

後処理

  1. temperaturewas heated
  2. temperatureAfter 20 hours reflux
  3. customthe excess amine and dimethylformamide were evaporated
  4. customthe residue was triturated with water
  5. filtrationfiltered
  6. washwashed with water
  7. customdried
  8. customRecrystallization from ethyl acetate/petroleum ether
  9. customgave pure product

出典と根拠

ORDレコード
ord-a8f31c3f69e44f889459e4fbf80bb158
出典データセット
uspto-grants-1998_03
特許番号
US05733914

関連ノート

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