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

HRID 359168

반응식

HRID 359168 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 82262Ethyl 3,3-dimethylpent-4-enoate수율 52%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-df5d0589e06c4d5380dc79a928de4c09
출처 데이터셋
uspto-grants-1991_03
특허 번호
US04999451

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