Benzaldehyde → HCID 54070128, 화합물

HRID 1247939노트

반응식

HRID 1247939 반응식
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([CH:15]=1)[C:7](=[O:14])[C:8]1[CH2:13][CH2:12][CH2:11][C:9]=1[N:10]=2.[CH:16](=O)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.C[O-].[Na+]>CO>[CH:16](=[C:11]1[C:9]2[N:10]=[C:5]3[CH:4]=[CH:3][C:2]([CH3:1])=[CH:15][N:6]3[C:7](=[O:14])[C:8]=2[CH2:13][CH2:12]1)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

참가 물질

5

반응물 3

HCID 240BenzaldehydeHCID 10942334Sodium MethoxideHCID 124855822,3-Dihydro-7-methylcyclopenta[d]pyrido[1,2-alpha]pyrimidin-10(1H)-one

생성물 1

HCID 54070128HCID 54070128, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

7-methyl-1,2,3,10-tetrahydro-cyclopenta[d]pyrido[1,2-a]pyrimidine-10-one (5 g) was reacted with benzaldehyde (13.2 g) in methanol (200 ml) in the presence of sodium methoxide (6.8 g) at reflux temperature for 96 hours. After cooling and concentration in vacuo to a small volume the precipitate was filtered and washed with water until neutral; crystallization from CH2Cl2 /methanol gave 3-benzylidene-7-methyl-1,2,3,10-tetrahydro-cyclopenta[d]pyrido[1,2-a]pyrimidine-10-one, m.p. 197°-199° C., NMR (CDCl3) δ ppm: 2.45 (s) (3H, CH3), 3.10 (bs) (4H, C-1 and C-2 protons), 7.2-7.7 (m) (8H, =CH-- and C-5 and C-6 and phenyl protons), 8.80 (bs) (1H, C-8 proton).

후처리

  1. temperatureat reflux temperature for 96 hours
  2. temperatureAfter cooling
  3. concentrationconcentration in vacuo to a small volume the precipitate
  4. filtrationwas filtered
  5. washwashed with water until neutral
  6. customcrystallization from CH2Cl2 /methanol

출처 및 근거

ORD 기록
ord-5e467be65e4944dabed7ec924b2ca33a
출처 데이터셋
uspto-grants-1985_06
특허 번호
US04521419

반응 노트

불러오는 중…