Phosphorus oxychloride → HCID 22011950、化合物

HRID 566389ノート

反応式

HRID 566389 の反応式
[CH3:1][C:2]1[O:6][C:5]([C:7]2[N:17]=[CH:16][C:10]3[N:11]=[CH:12][NH:13][C:14](=O)[C:9]=3[CH:8]=2)=[N:4][N:3]=1.P(Cl)(Cl)([Cl:20])=O>>[Cl:20][C:14]1[C:9]2[CH:8]=[C:7]([C:5]3[O:6][C:2]([CH3:1])=[N:3][N:4]=3)[N:17]=[CH:16][C:10]=2[N:11]=[CH:12][N:13]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 135817447HCID 135817447、化合物

生成物 1

HCID 22011950HCID 22011950、化合物

実験手順

6-(5-Methyl-1,3,4-oxadiazol-2-yl)-pyrido[3,4-d]pyrimidin-4-one (0.5 g) was treated with phosphorus oxychloride at room temperature under N2. After 1 hour at room temperature and 1 hour at 50° C., the mixture was concentrated in vacuo, azeotroping with toluene, then taken up in ethyl acetate, washed with sodium bicarbonate solution, dried and concentrated in vacuo to give the title compound (0.17 g) as an orange solid; δH CDCl3 9.68 (1H,s), 9.30 (1H,s), 8.96 (1H,s), 2.75 (3H,s); m/z (M+1+)248.

後処理

  1. concentration1 hour at 50° C., the mixture was concentrated in vacuo
  2. customazeotroping with toluene
  3. washwashed with sodium bicarbonate solution
  4. customdried
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-8a0d1750a8984fbcacad836ffbe7c7ed
出典データセット
uspto-grants-2001_01
特許番号
US06174889B1

反応ノート

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