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

HRID 1741615노트

반응식

HRID 1741615 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 1140Toluene용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-4656e1e58d284c8c94efb3e0cb10f85c
출처 데이터셋
uspto-grants-1994_08
특허 번호
US05334576

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