Acetic Anhydride → N-[6-(2,6-dichlorophenyl)-8-methyl-7-oxo-7H,8H-pyrido[2,3-d]pyrimidin-2-yl]acetamide

HRID 53624

반응식

HRID 53624 반응식
[NH2:1][C:2]1[N:3]=[CH:4][C:5]2[CH:11]=[C:10]([C:12]3[C:17]([Cl:18])=[CH:16][CH:15]=[CH:14][C:13]=3[Cl:19])[C:9](=[O:20])[N:8]([CH3:21])[C:6]=2[N:7]=1.[C:22](OC(=O)C)(=[O:24])[CH3:23]>>[Cl:18][C:17]1[CH:16]=[CH:15][CH:14]=[C:13]([Cl:19])[C:12]=1[C:10]1[C:9](=[O:20])[N:8]([CH3:21])[C:6]2[N:7]=[C:2]([NH:1][C:22](=[O:24])[CH3:23])[N:3]=[CH:4][C:5]=2[CH:11]=1

참가 물질

3

반응물 2

HCID 7918Acetic AnhydrideHCID 53278642-amino-6-(2,6-dichlorophenyl)-8-methyl-7H,8H-pyrido[2,3-d]pyrimidin-7-one

생성물 1

HCID 5327865N-[6-(2,6-dichlorophenyl)-8-methyl-7-oxo-7H,8H-pyrido[2,3-d]pyrimidin-2-yl]acetamide

반응 조건

온도
25 °C

실험 절차

A mixture of 64.2 mg (0.20 mmol) of 2-amino-6-(2,6-dichlorophenyl)-8-methyl-pyrido[2,3-d]pyrimidin-7(8H)-one (from Example 12) and 1 mL of acetic anhydride was heated to reflux. The resulting solution was maintained at reflux for 20 minutes and concentrated at atmospheric pressure to about 0.25 mL volume. The solution was cooled to 25° C. and diluted with diethyl ether (1 mL). The separated crystals were filtered and washed with diethyl ether to provide N-[6-(2,6-dichlorophenyl)-8-methyl-7-oxo-7,8-dihydro-pyrido[2,3-d]pyrimidin-2-yl]acetamide, wt 44.0 mg; mp 258°-260° C.; MS (CI) 363 (M+ +1).

후처리

  1. temperaturewas heated to reflux
  2. temperatureThe resulting solution was maintained
  3. temperatureat reflux for 20 minutes
  4. concentrationconcentrated at atmospheric pressure to about 0.25 mL volume
  5. additiondiluted with diethyl ether (1 mL)
  6. filtrationThe separated crystals were filtered
  7. washwashed with diethyl ether

출처 및 근거

ORD 기록
ord-26a020e1e80a4d4c857431a3c9c2b02f
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05620981

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