Acetaldehyde → 2,2,6-Trimethyl-5-isopropenyltetrahydropyran

HRID 885771노트

반응식

HRID 885771 반응식
[CH:1](=O)[CH3:2].B(F)(F)F.CCOCC.[CH3:13][C:14]([OH:22])([CH2:16][CH2:17][CH:18]=[C:19]([CH3:21])[CH3:20])[CH3:15]>C(OCC)C>[CH3:13][C:14]1([CH3:15])[CH2:16][CH2:17][CH:18]([C:19]([CH3:21])=[CH2:20])[CH:1]([CH3:2])[O:22]1

참가 물질

5

반응물 3

HCID 177AcetaldehydeHCID 8000Boron trifluoride etherateHCID 801835-Hepten-2-ol, 2,6-dimethyl-

생성물 1

HCID 667338572,2,6-Trimethyl-5-isopropenyltetrahydropyran수율 55.9%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

반응 조건

온도
0 °C

실험 절차

42 g of acetaldehyde in 600 ml diethylether were placed in a 2 liter three-necked flask and cooled to 0° C. 140 g of a 48% solution of boron trifluoride diethyl etherate were then added and stirred for 10 minutes at 0° C. 124 g of 2,6-dimethyl-hept-5-en-2-ol dissolved in 100 ml diethyl ether were droppered into the reaction solution at 0° C. Once addition was complete stirring continued for a further hour at 0° C. followed by heating to room temperature. Once the reaction solution had been stirred for 12 hours at room temperature, quenching was carried out with saturated ammonium chloride solution (500 ml) and following conditioning of the raw product obtained distillation was performed via a 30 cm packed column. 82 g of 2,2,6-trimethyl-5-isopropenyltetrahydropyran with a purity of 98% were obtained (55% of theoretical yield).

후처리

  1. customwere droppered into the reaction solution at 0° C
  2. additionOnce addition
  3. stirringwas complete stirring
  4. waitcontinued for a further hour at 0° C.
  5. temperatureby heating to room temperature
  6. stirringOnce the reaction solution had been stirred for 12 hours at room temperature
  7. customquenching
  8. customobtained
  9. distillationdistillation

출처 및 근거

ORD 기록
ord-4430f0f9d19c460b8f03ee52d92cc6a6
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08242289B2

반응 노트

불러오는 중…