Ethanol → 3-Bromo-4-ethoxybut-3-EN-2-one

HRID 280757노트

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HRID 280757 반응식
[CH2:1](O)[CH3:2].[Br:4][C:5](=[CH:9][OH:10])[C:6](=[O:8])[CH3:7]>C1(C)C=CC=CC=1>[Br:4][C:5](=[CH:9][O:10][CH2:1][CH3:2])[C:6](=[O:8])[CH3:7]

참가 물질

4

반응물 2

HCID 702EthanolHCID 573587893-Buten-2-one, 3-bromo-4-hydroxy-

생성물 1

HCID 534237433-Bromo-4-ethoxybut-3-EN-2-one수율 100%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of 400 ml absolute ethanol and 60 ml toluene was heated to reflux and 20 ml of azeotrope was removed via a Dean Stark trap. To the ethanol-toluene solution was added 33.0 g (0.2 mol) of 3-bromo-4-hydroxy-3-buten-2-one and reflux was continued for 2 hours during which period three aliquots of 20 ml of ethanol-toluene were removed via the trap. The solution was concentrated in vacuo to give 38.6 g (100%) of 3-bromo-4-ethoxy-3-buten-2-one as a mobile oil. nmr (DMSOd-6) (δ): 8.21 (s, 1H); 4.23 (g, 2H); 2.33 (s, 3H); 1.31 (s, 3H).

후처리

  1. temperaturewas heated
  2. temperatureto reflux
  3. custom20 ml of azeotrope was removed via a Dean Stark trap
  4. temperaturereflux
  5. customwere removed via the trap
  6. concentrationThe solution was concentrated in vacuo

출처 및 근거

ORD 기록
ord-c5207f141af54b8a9b9c89eef0e61fb7
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04590299

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