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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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2-Methyl-3-buten-2-ol → Methyl 5-methyl-4-hexenoate

HRID 45981
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HRID 45981 반응식
[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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

HCID 10909672Methyl 5-methyl-4-hexenoate수율 271.5%

시약·촉매·용매 1

HCID 1032Propionic Acid촉매

반응 조건

온도
115 °C

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-5daff547d48542a8a1e8915e60d7d5fe
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08541606B2

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