Water → 2,3-Dihydro-5-methoxy-1,4-benzodioxin

HRID 1440818

反応式

HRID 1440818 の反応式
[CH3:1][O:2][C:3]1[CH:9]=[CH:8][CH:7]=[C:5]([OH:6])[C:4]=1[OH:10].Br[CH2:12][CH2:13]Br.C(=O)([O-])[O-].[K+].[K+].O>OCC(CO)O.[Cu]>[CH3:1][O:2][C:3]1[C:4]2[O:10][CH2:13][CH2:12][O:6][C:5]=2[CH:7]=[CH:8][CH:9]=1

参加物

7

反応物 4

HCID 962WaterHCID 78391,2-DibromoethaneHCID 11430Potassium CarbonateHCID 136223-Methoxycatechol

生成物 1

HCID 743712,3-Dihydro-5-methoxy-1,4-benzodioxin

試薬・触媒・溶媒 2

HCID 23978Copper触媒HCID 753Glycerol溶媒

反応条件

温度
110 °C

実験手順

A heterogeneous mixture containing 1.42 mol of 3-methoxycatechol, 1.57 mol of 1,2-dibromoethane, 1.42 mol of potassium carbonate and 4 g of copper powder in 150 ml of glycerol is heated at 110° C. for 15 hours. After cooling, the mixture is poured into 1 l of water. The aqueous phase is extracted with ethyl ether. The ether phases are then washed with 1N sodium hydroxide, dried and evaporated, and give the expected product.

後処理

  1. temperatureAfter cooling
  2. extractionThe aqueous phase is extracted with ethyl ether
  3. washThe ether phases are then washed with 1N sodium hydroxide
  4. customdried
  5. customevaporated

出典と根拠

ORDレコード
ord-3e0e7df9f5d944b48480b7e0c5e1eedc
出典データセット
uspto-grants-1996_03
特許番号
US05500443

関連ノート

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