Benzene → 1-[Bis(hydroxymethyl)-methyl]-6,7-dimethoxy-3,4-dihydroisoquinoline

HRID 542191

反応式

HRID 542191 の反応式
[CH2:1]=[O:2].C1C=CC=CC=1.[CH3:9][C:10]1[C:19]2[C:14](=[CH:15][C:16]([O:22][CH3:23])=[C:17]([O:20][CH3:21])[CH:18]=2)[CH2:13][CH2:12][N:11]=1.C[CH2:25][O-:26].[Na+]>>[OH:2][CH2:1][CH:9]([CH2:25][OH:26])[C:10]1[C:19]2[C:14](=[CH:15][C:16]([O:22][CH3:23])=[C:17]([O:20][CH3:21])[CH:18]=2)[CH2:13][CH2:12][N:11]=1

参加物

5

反応物 4

HCID 241BenzeneHCID 712FormaldehydeHCID 226523,4-Dihydro-6,7-dimethoxy-1-methylisoquinolineHCID 2723922Sodium ethoxide

生成物 1

HCID 136966801-[Bis(hydroxymethyl)-methyl]-6,7-dimethoxy-3,4-dihydroisoquinoline

実験手順

To a solution of 2.5 moles of paraformaldehyde in 500 ml. of benzene 1 mole (205.3 g) of 1-methyl-6,7-dimethoxy-3,4-dihydroisoquinoline and subsequently freshly prepared sodium ethylate (1 g sodium+50 ml ethanol) are added at room temperature, with stirring. The reaction mixture is refluxed for 4 hours. The mixture is then evaporated under reduced pressure, and the obtained crystalline material is recrystallized from a mixture of acetone and ether. The aimed compound is obtained which has the same melting point as the product prepared in Example 1.

後処理

  1. temperatureThe reaction mixture is refluxed for 4 hours
  2. customThe mixture is then evaporated under reduced pressure
  3. customthe obtained crystalline material is recrystallized from a mixture of acetone and ether

出典と根拠

ORDレコード
ord-275bef7252a34716816043ec5c21bea5
出典データセット
uspto-grants-1987_04
特許番号
US04656179

関連ノート

読み込み中…