2-Methyl-3-buten-2-ol → Methyl 5-methyl-4-hexenoate

HRID 45981

反応式

HRID 45981 の反応式
[CH:1]([C:3](O)([CH3:5])[CH3:4])=[CH2:2].[C:7](OC)([O:11]C)([O:9][CH3:10])[CH3:8]>C(O)(=O)CC>[CH3:4][C:3]([CH3:5])=[CH:1][CH2:2][CH2:8][C:7]([O:9][CH3:10])=[O:11]

参加物

4

反応物 2

HCID 82572-Methyl-3-buten-2-olHCID 15050Trimethyl orthoacetate

生成物 1

HCID 10909672Methyl 5-methyl-4-hexenoate収率 271.5%

試薬・触媒・溶媒 1

HCID 1032Propionic Acid触媒

反応条件

温度
115 °C

実験手順

A distillation column-provided four-necked flask having a volume of one liter, which was equipped with a dropping funnel, a thermometer, a stirring device and a reflux ratio regulator, was charged with 50.0 g (580.5 mmoles) of 2-vinyl-2-propanol, 139.5 g (1,161.0 mmoles) of trimethyl orthoacetate and 1.3 g (17.4 mmoles) of propionic acid, and the internal temperature was raised to 115° C. Heating was continued for 12 hours while removing a fraction of not higher than 65° C. from a column top of the distillation column. After confirming the disappearance of 2-vinyl-2-propanol by a gas chromatographic analysis of the reaction solution, the reaction solution was distilled in vacuo. Fractions of from 60 to 65° C./1.2 kPa were collected to obtain 62.2 g (437.1 mmoles) of methyl 5-methyl-4-hexenate. The yield was 75.3%.

後処理

  1. distillationA distillation
  2. customcolumn-provided four-necked flask
  3. customwas equipped with a dropping funnel
  4. temperatureHeating
  5. customwhile removing a fraction of not higher than 65° C.
  6. distillationfrom a column top of the distillation column
  7. distillationthe reaction solution was distilled in vacuo
  8. customFractions of from 60 to 65° C./1.2 kPa were collected

出典と根拠

ORDレコード
ord-5daff547d48542a8a1e8915e60d7d5fe
出典データセット
uspto-grants-2013_09
特許番号
US08541606B2

関連ノート

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