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

HRID 3186

반응식

HRID 3186 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
110 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a8f31c3f69e44f889459e4fbf80bb158
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05733914

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