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2-Thiophenecarboxaldehyde → 3,4-Dimethoxy-alpha-methylbenzenemethanamine

HRID 1585818
ノート
印刷プレビュー

反応式

HRID 1585818 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C@@H:11]([NH2:13])[CH3:12])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].S1C=CC=C1C=O>ClCCl>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:11]([NH2:13])[CH3:12])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]
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

4

反応物 2

HCID 73642-ThiophenecarboxaldehydeHCID 376091(1s)-1-(3,4-Dimethoxyphenyl)ethanamine

生成物 1

HCID 31592433,4-Dimethoxy-alpha-methylbenzenemethanamine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
20 °C

実験手順

To a solution of 43.8 g of (S)-1-(3,4-dimethoxyphenyl)ethylamine in 400 cm3 of dichloromethane are added, with stirring at a temperature in the region of 20° C., 16.8 cm3 of 2-thiophenecarboxaldehyde and 35 g of 4Å molecular sieves. The reaction mixture is stirred for 16 hours at a temperature in the region of 20° C., and then filtered through a sinter funnel containing Celite. The sinter funnel is washed with 3 times 50 cm3 of dichloromethane and the filtrates are combined and then concentrated to dryness under reduced pressure (2.7 kPa) at 40° C. 45.95 g of (S)-N-(2-thienyl)-methylidene]-[1-(3,4-dimethoxyphenyl)ethylamine are thus obtained in the form of a colourless oil for which the characteristics are the following:

後処理

  1. filtrationfiltered through a sinter funnel
  2. additioncontaining Celite
  3. washThe sinter funnel is washed with 3 times 50 cm3 of dichloromethane
  4. concentrationconcentrated to dryness under reduced pressure (2.7 kPa) at 40° C

出典と根拠

ORDレコード
ord-c03228919f6f4c2881d27cfbf7c44928
出典データセット
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05939561

反応ノート

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