Benzaldehyde → HCID 54070128、化合物

HRID 1247939ノート

反応式

HRID 1247939 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 54070128HCID 54070128、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-5e467be65e4944dabed7ec924b2ca33a
出典データセット
uspto-grants-1985_06
特許番号
US04521419

反応ノート

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