Phosphorus oxychloride → 3-Benzyl-5-chloro-6,8-dimethylpyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione

HRID 1660889ノート

反応式

HRID 1660889 の反応式
[CH2:1]([N:8]1[C:13](=[O:14])[C:12]2[C:15](O)=[C:16]([CH3:21])[C:17](=[O:20])[N:18]([CH3:19])[C:11]=2[N:10]=[CH:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O=P(Cl)(Cl)[Cl:25]>>[CH2:1]([N:8]1[C:13](=[O:14])[C:12]2[C:15]([Cl:25])=[C:16]([CH3:21])[C:17](=[O:20])[N:18]([CH3:19])[C:11]=2[N:10]=[CH:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 598230503-Benzyl-5-hydroxy-6,8-dimethylpyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione

生成物 1

HCID 598230643-Benzyl-5-chloro-6,8-dimethylpyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione

実験手順

3-Benzyl-5-hydroxy-6,8-dimethylpyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione (5.5 g, 18.5 mmol) was dissolved in excess POCl3 (50 mL) and heated at reflux for 1 hour. POCl3 was removed in vacuo and the residue dissolved in DCM then quickly washed with saturated sodium bicarbonate solution until neutral pH was observed. The organic layer was dried over MgSO4 and evaporated to dryness to give 7.3 g of the title compound as an impure reddish brown solid. [M+H] calc'd for C16H14ClN3O2, 315; found, 315.

後処理

  1. temperatureheated
  2. temperatureat reflux for 1 hour
  3. customPOCl3 was removed in vacuo
  4. dissolutionthe residue dissolved in DCM
  5. washthen quickly washed with saturated sodium bicarbonate solution until neutral pH
  6. dry with materialThe organic layer was dried over MgSO4
  7. customevaporated to dryness

出典と根拠

ORDレコード
ord-8fa6562cb3e94b15b203742094a97700
出典データセット
uspto-grants-2011_10
特許番号
US08030317B2

反応ノート

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