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

HRID 542192

反応式

HRID 542192 の反応式
[CH3:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=2)[CH2:5][CH2:4][N:3]=1.[CH2:16]=[O:17].[CH3:18][O-:19].[Na+]>CO>[OH:17][CH2:16][CH:1]([CH2:18][OH:19])[C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=2)[CH2:5][CH2:4][N:3]=1

参加物

5

反応物 3

HCID 712FormaldehydeHCID 226523,4-Dihydro-6,7-dimethoxy-1-methylisoquinolineHCID 10942334Sodium Methoxide

生成物 1

HCID 136966801-[Bis(hydroxymethyl)-methyl]-6,7-dimethoxy-3,4-dihydroisoquinoline収率 79%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To 1 mole (205.3 g) of 1-methyl-6,7-dimethoxy-3,4-dihydroisoquinoline 100 ml of a 30% aqueous formaldehyde solution and then freshly prepared sodium methylate (1 g of sodium+50 ml of methanol) are added. The mixture is then slightly refluxed in 500 ml of methanol for 2 hours. The reaction mixture is evaporated under reduced pressure and the obtained crystalline product is recrystallized from a mixture of acetone and ether. The aimed compound is obtained with the same melting point as the product of Example 1.

後処理

  1. customThe reaction mixture is evaporated under reduced pressure
  2. customthe obtained crystalline product is recrystallized from a mixture of acetone and ether

出典と根拠

ORDレコード
ord-26e3d656308d441283e590390f0983fc
出典データセット
uspto-grants-1987_04
特許番号
US04656179

関連ノート

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