홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Water → Diethyl-2-ethyl-2-(3-cyclohexylpropyl)-malonate

HRID 27305
노트
인쇄 미리보기

반응식

HRID 27305 반응식
[Na].[CH2:2]([CH:4]([C:10]([O:12][CH2:13][CH3:14])=[O:11])[C:5]([O:7][CH2:8][CH3:9])=[O:6])[CH3:3].[Na][C:16](C(CC)(CC)C)(C([O-])=O)[C:17]([O-])=O.O.[C:30]1([CH3:37])[C:31](C)=[CH:32][CH:33]=[CH:34][CH:35]=1>C1(C)C=CC=CC=1>[CH2:8]([O:7][C:5](=[O:6])[C:4]([CH2:16][CH3:17])([CH2:2][CH2:3][CH2:37][CH:30]1[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]1)[C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH3:9]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 962WaterHCID 7237O-XyleneHCID 8610Diethyl ethylmalonateHCID 5360545SodiumHCID 178443961HCID 178443961, 화합물

생성물 1

HCID 23344469Diethyl-2-ethyl-2-(3-cyclohexylpropyl)-malonate

시약·촉매·용매 1

HCID 1140
Toluene
용매

반응 조건

온도
150 °C

실험 절차

Sodium metal (3.16 g, 0.137 g/atom) was dispersed by heating with rapid stirring in 80 ml of dry xylene at 110° to 120° C. The mixture was cooled and the xylene was removed with a filter stick. Dry toluene (300 ml distilled from calcium hydride) was added thereto and followed by the addition of 28.17 g (0.149 mole) of diethyl ethylmalonate. This mixture was slowly heated to 150° C. 3-Cyclohexylpropyl-1-tosylate (28.3 g, 1.1956 mole; prepared by Example 10A) was dissolved in 80 ml of dry toluene. This solution was then added to the sodiodiethylethylmalonate above and the mixture was stirred at 150° C. for 10 hr. The mixture was cooled and poured into 500 ml of water. The phases were separated and the aqueous phase was extracted with 500 ml (2×250 ml) of ether. The ether extract was washed with 250 ml of saturated sodium chloride solution, dried over a anhydrous magnesium sulfate and filtered. The solvents were removed in vacuo. The product was distilled at reduced pressure to yield 19.4 g of the title compound having the following physical characteristics:

후처리

  1. temperatureby heating
  2. temperatureThe mixture was cooled
  3. customthe xylene was removed with a filter stick
  4. additionDry toluene (300 ml distilled from calcium hydride) was added
  5. temperatureThe mixture was cooled
  6. customThe phases were separated
  7. extractionthe aqueous phase was extracted with 500 ml (2×250 ml) of ether
  8. extractionThe ether extract
  9. washwas washed with 250 ml of saturated sodium chloride solution
  10. dry with materialdried over a anhydrous magnesium sulfate
  11. filtrationfiltered
  12. customThe solvents were removed in vacuo
  13. distillationThe product was distilled at reduced pressure

출처 및 근거

ORD 기록
ord-15489f8eb5c34cd1b606a254e022aeb4
출처 데이터셋
uspto-grants-1980_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04220795

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트