Phosphorus oxychloride → HCID 59427361、化合物

HRID 1042797ノート

反応式

HRID 1042797 の反応式
[CH3:1][C:2]1[N:7]=[C:6]([C:8]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[C:11](=O)[NH:10][N:9]=2)[CH:5]=[CH:4][CH:3]=1.O=P(Cl)(Cl)[Cl:21]>>[Cl:21][C:11]1[C:12]2[C:17](=[CH:16][CH:15]=[CH:14][CH:13]=2)[C:8]([C:6]2[CH:5]=[CH:4][CH:3]=[C:2]([CH3:1])[N:7]=2)=[N:9][N:10]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 67017182HCID 67017182、化合物

生成物 1

HCID 59427361HCID 59427361、化合物

反応条件

温度
0 °C

実験手順

A dry RBF set up with stirring bar and reflux condenser was charged with 4-(6-methylpyridin-2-yl)phthalazin-1(2H)-one (780 mg, 3.29 mmol) and POCl3 (10.7 ml, 115 mmol). This was stirred under reflux for 18 h. Excess POCl3 was removed under vacuum with an aid of toluene. The residue was cooled to 0° C. and basified with cold 6 N NaOH until pH=9. Occasionally, ice was added to keep the mixture cold to prevent the hydrolysis. Stirring, agitation, and sonication eventually provided a solid material at basic pH. The solids were filtered, washed with ample amount of water and dried under vacuum to afford a white solid. MS Calcd for C14H10ClN3: [M]+=255. Found: [M+H]+=256.

後処理

  1. temperaturereflux condenser
  2. stirringThis was stirred
  3. temperatureunder reflux for 18 h
  4. customExcess POCl3 was removed under vacuum with an aid of toluene
  5. additionOccasionally, ice was added
  6. customthe hydrolysis
  7. stirringStirring
  8. customagitation, and sonication
  9. customeventually provided a solid material at basic pH
  10. filtrationThe solids were filtered
  11. washwashed with ample amount of water
  12. customdried under vacuum
  13. customto afford a white solid

出典と根拠

ORDレコード
ord-3011a51f7cfc4ce9ba5372a863ed0cc9
出典データセット
uspto-grants-2013_10
特許番号
US08557816B2

反応ノート

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