3,4,5-Trimethoxybenzaldehyde → HCID 21853792、化合物

HRID 1580938

反応式

HRID 1580938 の反応式
C[O-].[Na+].[CH3:4][C:5]1[N:6]=[C:7]2[C:16]([CH3:17])=[CH:15][CH:14]=[CH:13][N:8]2[C:9](=[O:12])[C:10]=1[CH3:11].[CH3:18][O:19][C:20]1[CH:21]=[C:22]([CH:25]=[C:26]([O:30][CH3:31])[C:27]=1[O:28][CH3:29])[CH:23]=O>C(O)C>[CH3:11][C:10]1[C:9](=[O:12])[N:8]2[CH:13]=[CH:14][CH:15]=[C:16]([CH3:17])[C:7]2=[N:6][C:5]=1/[CH:4]=[CH:23]/[C:22]1[CH:25]=[C:26]([O:30][CH3:31])[C:27]([O:28][CH3:29])=[C:20]([O:19][CH3:18])[CH:21]=1

参加物

5

反応物 3

HCID 68583,4,5-TrimethoxybenzaldehydeHCID 10942334Sodium MethoxideHCID 123397192,3,9-Trimethyl-4H-pyrido[1,2-a]pyrimidin-4-one

生成物 1

HCID 21853792HCID 21853792、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 1.3g of sodium methoxide in 75ml of absolute ethanol is added 2.0g of 2,3,9-trimethyl-4H-pyrido-[1,2-a]pyrimidin-4-one, followed by 4.0g of 3,4,5-trimethoxybenzaldehyde. The mixture is stirred and heated under reflux for 89 hours. The reaction mixture is cooled, the solid is filtered, washed with 20ml of ether and 25ml of water, dried, and recrystallized from 75ml of acetonitrile to yield the title compound, melting point 218°-219°C dec.

後処理

  1. temperatureheated
  2. temperatureunder reflux for 89 hours
  3. temperatureThe reaction mixture is cooled
  4. filtrationthe solid is filtered
  5. washwashed with 20ml of ether and 25ml of water
  6. customdried
  7. customrecrystallized from 75ml of acetonitrile

出典と根拠

ORDレコード
ord-d89cf70173b24f458c8421a5b15a938f
出典データセット
uspto-grants-1976_01
特許番号
US03935197

関連ノート

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