p-Toluidine → 6-(2,6-Dichlorophenyl)-8-methyl-3-p-tolylamino-8H-pyrido[2,3-d]pyrimidin-7-one

HRID 3198

반응식

HRID 3198 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:22](=[O:23])[N:21]([CH3:24])[C:12]2[N:13]=[C:14](S(C)(=O)=O)[N:15]=[CH:16][C:11]=2[CH:10]=1.[CH3:25][C:26]1[CH:32]=[CH:31][C:29]([NH2:30])=[CH:28][CH:27]=1>>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:22](=[O:23])[N:21]([CH3:24])[C:12]2=[N:13][CH2:14][N:15]([NH:30][C:29]3[CH:31]=[CH:32][C:26]([CH3:25])=[CH:27][CH:28]=3)[CH:16]=[C:11]2[CH:10]=1

참가 물질

3

반응물 2

HCID 7813p-ToluidineHCID 105961576-(2,6-Dichlorophenyl)-8-methyl-2-methylsulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one

생성물 1

HCID 867523446-(2,6-Dichlorophenyl)-8-methyl-3-p-tolylamino-8H-pyrido[2,3-d]pyrimidin-7-one

반응 조건

온도
180 °C

실험 절차

A mixture of 0.113 g (0.29 mmol) of 6-(2,6-dichlorophenyl)-2-methanesulfonyl-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 39 and 0.50 g (4.70 mmol) of 4-methylaniline was heated, with stirring, in a 180° C. oil bath. The resulting solution was heated for 10 minutes. Much of the excess 4-methylaniline was evaporated at reduced pressure. The remainder was dissolved in 1 mL of ethyl acetate. The crystals that separated from the dark solution were filtered and washed with 2 mL of ethyl acetate and then ether; wt 0.111 g. Recrystallization from ethyl acetate gave pure product; wt 0.050 g; mp 243°-245° C.

후처리

  1. temperaturewas heated
  2. temperatureThe resulting solution was heated for 10 minutes
  3. customMuch of the excess 4-methylaniline was evaporated at reduced pressure
  4. dissolutionThe remainder was dissolved in 1 mL of ethyl acetate
  5. customThe crystals that separated from the dark solution
  6. filtrationwere filtered
  7. washwashed with 2 mL of ethyl acetate
  8. customRecrystallization from ethyl acetate
  9. customgave pure product

출처 및 근거

ORD 기록
ord-7c0d2f4521364c5dbc8d4b38d2935639
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05733914

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