Morpholine → 1-Morpholino-1-(thiophen-3-yl)-ethylene

HRID 358851ノート

反応式

HRID 358851 の反応式
[C:1]([C:4]1[CH:8]=[CH:7][S:6][CH:5]=1)(=O)[CH3:2].[NH:9]1[CH2:14][CH2:13][O:12][CH2:11][CH2:10]1>C1CCCCC1.[Ti](Cl)(Cl)(Cl)Cl>[O:12]1[CH2:13][CH2:14][N:9]([C:1]([C:4]2[CH:8]=[CH:7][S:6][CH:5]=2)=[CH2:2])[CH2:10][CH2:11]1

参加物

5

反応物 2

HCID 8083MorpholineHCID 151161-(Thiophen-3-yl)ethanone

生成物 1

HCID 200671861-Morpholino-1-(thiophen-3-yl)-ethylene収率 31.4%

試薬・触媒・溶媒 2

HCID 24193Titanium Tetrachloride触媒HCID 8078Cyclohexane溶媒2 回

実験手順

A solution of 57 g of titanium tetrachloride (TiCl4) in 100 ml of cyclohexane is added dropwise to a stirred solution of 75 g of 3-acetylthiophene and 160 g of morpholine in a liter of cyclohexane. When the addition is complete, the reaction mixture is further stirred at room temperature for 12 hours, then the precipitate is filtered off and the filtrate is concentrated by evaporation. The residue is distilled and has a boiling point of 98°/0.04 millibar. In this manner 36.5 g of 1-morpholino-1-(thiophen-3-yl)-ethylene are obtained in the form of a colourless oil.

後処理

  1. additionWhen the addition
  2. filtrationthe precipitate is filtered off
  3. concentrationthe filtrate is concentrated by evaporation
  4. distillationThe residue is distilled

出典と根拠

ORDレコード
ord-c3092dfd59cb497f892d6308700bccef
出典データセット
uspto-grants-1991_03
特許番号
US04997947

反応ノート

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