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

HRID 280757ノート

反応式

HRID 280757 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 534237433-Bromo-4-ethoxybut-3-EN-2-one収率 100%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-c5207f141af54b8a9b9c89eef0e61fb7
出典データセット
uspto-grants-1986_05
特許番号
US04590299

反応ノート

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