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Potassium Hydroxide → 6-Methoxy-1-methyl-3,4-dihydroisoquinoline

HRID 275895
ノート
印刷プレビュー

反応式

HRID 275895 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:9][CH2:10][NH:11][C:12](=O)[CH3:13])[CH:6]=[CH:7][CH:8]=1.[OH-].[K+]>>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:6](=[CH:7][CH:8]=1)[C:12]([CH3:13])=[N:11][CH2:10][CH2:9]2
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 14797Potassium HydroxideHCID 10330235N-[2-(3-methoxyphenyl)ethyl]acetamide

生成物 1

HCID 138591866-Methoxy-1-methyl-3,4-dihydroisoquinoline収率 93.4%

反応条件

温度
110 °C

実験手順

A mixture soultion of polyphosphoric acid (61.4 ml, 0.66 mol) and phosphorouspentoxide(28.0 g, 0.2 mol) was heated to 90° C. N-(3-methoxyphenylethyl) acetamide (63.6 g, 0.33 mol) was added to the mixture solution and then stirred for 2 hours at 110° C. The reaction mixture was poured into ice water, adjusted to alkali with potassium hydroxide, and then extracted with ethyl ether. The extract was dried over anhydrous magnesium sulfate and concentrated under a reduces pressure. The resulting residue was purified by a silica gel column chromatography, using a solution of methanol and dichloromethane (1:20) as a eluent, to give 54.0 g of the titled compound.

後処理

  1. extractionextracted with ethyl ether
  2. dry with materialThe extract was dried over anhydrous magnesium sulfate
  3. concentrationconcentrated under a reduces pressure
  4. customThe resulting residue was purified by a silica gel column chromatography

出典と根拠

ORDレコード
ord-02fafa00edc44bb78611cf51bfbf954a
出典データセット
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06352993B1

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート