Morpholine → 4-[2-(Thiophen-2-yl)ethenyl]morpholine

HRID 1741615ノート

反応式

HRID 1741615 の反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][CH:7]=O.[NH:9]1[CH2:14][CH2:13][O:12][CH2:11][CH2:10]1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1.C[O-].[Na+]>C1(C)C=CC=CC=1.O>[O:12]1[CH2:13][CH2:14][N:9]([CH:7]=[CH:6][C:2]2[S:1][CH:5]=[CH:4][CH:3]=2)[CH2:10][CH2:11]1

参加物

7

反応物 4

HCID 8083MorpholineHCID 521998p-Toluenesulfonic acid monohydrateHCID 64307222-(Thiophen-2-yl)acetaldehydeHCID 10942334Sodium Methoxide

生成物 1

HCID 540174394-[2-(Thiophen-2-yl)ethenyl]morpholine

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1140Toluene溶媒

実験手順

A mixture of 1.5 g of 2-thienylacetaldehyde, 1.4 mL of morpholine, and 0.012 g of p-toluenesulfonic acid hydrate in 7.5 mL of toluene is heated at reflux under a Dean-Stark Trap with azeotropic removal of water for 3 hours. The solution is cooled, neutralized by the addition of solid sodium methoxide, and concentrated in vacuo. The residue is taken up in toluene, filtered, and concentrated in vacuo to afford the desired enamine as an oil.

後処理

  1. temperatureis heated
  2. temperatureThe solution is cooled
  3. concentrationconcentrated in vacuo
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-4656e1e58d284c8c94efb3e0cb10f85c
出典データセット
uspto-grants-1994_08
特許番号
US05334576

反応ノート

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