Heptane → Methyl 6-bromohex-2-enoate

HRID 1513541ノート

反応式

HRID 1513541 の反応式
[CH3:1][O:2][C:3](=[O:10])[CH:4]=[CH:5][CH2:6][CH2:7][CH2:8]Cl.[Br-:11].[Li+].CCCCCCC>O>[CH3:1][O:2][C:3](=[O:10])[CH:4]=[CH:5][CH2:6][CH2:7][CH2:8][Br:11]

参加物

5

反応物 3

HCID 8900Heptane2 回HCID 82050Lithium BromideHCID 85444077HCID 85444077、化合物

生成物 1

HCID 53811689Methyl 6-bromohex-2-enoate収率 83%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

In an atmosphere of nitrogen, 6-chloro-2-hexenoic acid methyl ester (4Cl); 188.8 g {GC purity; 83.6%, pure amount; 157.9 g (0.971 mol)}, lithium bromide (126.5 g, 1.457 mol) and heptane (16 ml) were added to a 500 ml capacity flask, followed by stirring for 6 hours under heptane reflux. After completion of the reaction, heptane was added as an extraction solvent and water was added thereto to separate the organic layer. The solvent was evaporated under a reduced pressure using an evaporator, and then the residue was distilled under a reduced pressure (70 to 80° C./0.1 ton) to obtain 6-bromo-2-hexenoic acid methyl ester (4Br); 203.4 g {GC purity; 82.3%, pure amount (4Br); 167.5 g (0.809 mol, yield 83%/(4Cl)}.

後処理

  1. temperaturereflux
  2. additionwas added
  3. customto separate the organic layer
  4. customThe solvent was evaporated under a reduced pressure
  5. customan evaporator
  6. distillationthe residue was distilled under a reduced pressure (70 to 80° C./0.1 ton)

出典と根拠

ORDレコード
ord-fc2f0be483fc4e008a53d25faa8aa40b
出典データセット
uspto-grants-2012_07
特許番号
US08217192B2

反応ノート

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