3-Methyl-2-buten-1-OL → Ethyl 3,3-dimethylpent-4-enoate

HRID 359168

反応式

HRID 359168 の反応式
[CH3:1][C:2]([CH3:6])=[CH:3][CH2:4]O.[C:7]([O-:13])([O-])([O:9][CH2:10][CH3:11])[CH3:8]>C(O)C>[CH3:1][C:2]([CH3:6])([CH:3]=[CH2:4])[CH2:8][C:7]([O:9][CH2:10][CH3:11])=[O:13]

参加物

4

反応物 2

HCID 111733-Methyl-2-buten-1-OLHCID 86598186Ethyl ortho-acetate

生成物 1

HCID 82262Ethyl 3,3-dimethylpent-4-enoate収率 52%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 4.3 g of 3-methyl-2-buten-1-ol and 8.1 g of ethyl orthoacetate was heated with stirring. The temperature was increased slowly from room temperature to 165° over 2 hours, during which 2.21 g of ethanol was collected. The temperature was maintained at 165° for 26 hours, during which time an additional 1.52 g of ethanol was collected. The reaction mixture was then allowed to cool and diluted with diethyl ether. The ether solution was washed successively with dilute hydrochloric acid, saturated aqueous sodium bicarbonate and saturated aqueous sodium chloride. The washed solution was dried over magnesium sulfate and distilled to give 4.03 g (52% yield) of ethyl 3,3-dimethyl-4-pentenoate, b.p. 80°-85°/52 mm.

後処理

  1. temperaturewas heated
  2. customwas collected
  3. temperatureThe temperature was maintained at 165° for 26 hours, during which time an additional 1.52 g of ethanol
  4. customwas collected
  5. temperatureto cool
  6. additiondiluted with diethyl ether
  7. washThe ether solution was washed successively with dilute hydrochloric acid, saturated aqueous sodium bicarbonate and saturated aqueous sodium chloride
  8. dry with materialThe washed solution was dried over magnesium sulfate
  9. distillationdistilled

出典と根拠

ORDレコード
ord-df5d0589e06c4d5380dc79a928de4c09
出典データセット
uspto-grants-1991_03
特許番号
US04999451

関連ノート

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