Phosphorus oxychloride → HCID 22011950, 화합물

HRID 566389노트

반응식

HRID 566389 반응식
[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

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 135817447HCID 135817447, 화합물

생성물 1

HCID 22011950HCID 22011950, 화합물

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8a0d1750a8984fbcacad836ffbe7c7ed
출처 데이터셋
uspto-grants-2001_01
특허 번호
US06174889B1

반응 노트

불러오는 중…