6-Methoxy-3-pyridinylamine → 2-aminopyrido[2,3-d]pyrimidin-7(8H)-one 41

HRID 3214

반응식

HRID 3214 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.[NH2:25][C:26]1[CH:27]=[CH:28][C:29]([O:32][CH3:33])=[N:30][CH:31]=1>O>[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]([NH:25][C:26]3[CH:31]=[N:30][C:29]([O:32][CH3:33])=[CH:28][CH:27]=3)[N:15]=[CH:16][C:11]=2[CH:10]=1

참가 물질

4

반응물 2

HCID 811216-Methoxy-3-pyridinylamineHCID 105961576-(2,6-Dichlorophenyl)-8-methyl-2-methylsulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one

생성물 1

HCID 53278882-aminopyrido[2,3-d]pyrimidin-7(8H)-one 41

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
160 °C

실험 절차

A mixture of 0.155 g (0.40 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 (4.00 mmol) of 5-amino-2-methoxypyridine was heated, with stirring, in a 160° C. oil bath. The resulting solution was heated for 10 minutes and cooled to room temperature. Water (10 mL) was added to precipitate a gum. The mixture was decanted, and the remaining gum was triturated with 5 mL of water. The brown solid that developed was filtered, washed well with water, and dried; wt 0.135 g. Purification was effected by silica gel chromatography eluting with chloroform and then with ethyl acetate to obtain the fraction containing pure product. The eluent was concentrated to 2 mL volume. The crystals that separated on inducement were filtered and washed with 0.2 mL of ethyl acetate and then 0.5 mL of ether; wt 0.045 g; mp 233°-235° C.

후처리

  1. temperaturewas heated
  2. temperatureThe resulting solution was heated for 10 minutes
  3. temperaturecooled to room temperature
  4. customto precipitate a gum
  5. customThe mixture was decanted
  6. customthe remaining gum was triturated with 5 mL of water
  7. filtrationThe brown solid that developed was filtered
  8. washwashed well with water
  9. customdried
  10. customPurification
  11. washeluting with chloroform
  12. customwith ethyl acetate to obtain the fraction
  13. additioncontaining pure product
  14. concentrationThe eluent was concentrated to 2 mL volume
  15. customThe crystals that separated on inducement
  16. filtrationwere filtered
  17. washwashed with 0.2 mL of ethyl acetate

출처 및 근거

ORD 기록
ord-09f50aa656964facbcc08ceb73b76632
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05733914

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