Phenol → Methyl 3,3-dimethyl-4-pentenoate

HRID 1758560

反応式

HRID 1758560 の反応式
[C:1](OC)([O:5][CH3:6])([O:3]C)[CH3:2].[CH3:9][C:10]([CH3:14])=[CH:11][CH2:12]O.C1(O)C=CC=CC=1>CO>[CH3:9][C:10]([CH3:14])([CH:11]=[CH2:12])[CH2:2][C:1]([O:5][CH3:6])=[O:3]

参加物

5

反応物 3

HCID 996PhenolHCID 111733-Methyl-2-buten-1-OLHCID 15050Trimethyl orthoacetate

生成物 1

HCID 114129Methyl 3,3-dimethyl-4-pentenoate収率 40%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of trimethyl orthoacetate (120 g; 1 mole), 3-methylbut-2-enol (21.5 g; 0.25 mole) and phenol (1.4 g; 0.015 mole) was placed in a flask equipped with a stirrer and a 10 cm fractionating column packed with Fenske rings. The mixture was heated, with stirring, to a temperature of 95°-110° C. and maintained at this temperature for a period of 2 hours while the methanol formed was collected by distillation. The excess trimethyl orthoacetate was distilled from the reaction mixture over a period of 1 hour during which time the temperature of the reaction mixture was raised to 140°-145° C. The mixture was heated, with stirring, at a temperature of 140°-145° C. for a period of 20 hours and then the product was distilled to give methyl 3,3-dimethylpent-4-enoate (14.2 g; 40%), bp 95°-99° C. at 140 mm Hg.

後処理

  1. customwas placed in a flask
  2. customequipped with a stirrer
  3. temperatureThe mixture was heated
  4. customformed
  5. distillationwas collected by distillation
  6. distillationThe excess trimethyl orthoacetate was distilled from the reaction mixture over a period of 1 hour during which time the temperature of the reaction mixture
  7. temperaturewas raised to 140°-145° C
  8. temperatureThe mixture was heated
  9. stirringwith stirring, at a temperature of 140°-145° C. for a period of 20 hours
  10. distillationthe product was distilled

出典と根拠

ORDレコード
ord-6904aaa213394ffa9b2d100773f6d3ff
出典データセット
uspto-grants-1983_02
特許番号
US04374264

関連ノート

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