Iodoethane → 1,3,3-Trimethylbicyclo(2.2.1)hept-2-yl 3-methylbutanoate

HRID 2183429노트

반응식

HRID 2183429 반응식
I[CH2:2][CH3:3].[OH:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:7][CH:6]=1.C([O-])([O-])=O.[K+].[K+]>CC(C)=O>[CH2:2]([O:4][C:5]1[CH:6]=[CH:7][C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:9][CH:10]=1)[CH3:3]

참가 물질

5

반응물 3

HCID 6340IodoethaneHCID 71034-HydroxybiphenylHCID 11430Potassium Carbonate

생성물 1

HCID 2225171,3,3-Trimethylbicyclo(2.2.1)hept-2-yl 3-methylbutanoate수율 166%

시약·촉매·용매 1

HCID 180Acetone용매2회

실험 절차

Iodoethane (68.7 g, 35,57 mL, 440.6 mmol) was added to a suspension of 50 g (170.2 mmol) of 4-hydroxy-1,1′-biphenyl and 40.6 g (293.75 mmol) K2CO3 in 600 mL acetone. The resulting reaction mixture was stirred under reflux for 16 hours. After cooling to room temperature the acetone was removed under reduced pressure, the residue was dissolved in ethyl acetate and extracted with water. The aqueous layers where extracted 3 times with ethyl acetate, the combined organic phases dried (Na2SO4) and evaporated to yield 56 g of the desired compound as a colorless solid.

후처리

  1. customThe resulting reaction mixture
  2. temperatureunder reflux for 16 hours
  3. customwas removed under reduced pressure
  4. dissolutionthe residue was dissolved in ethyl acetate
  5. extractionextracted with water
  6. extractionThe aqueous layers where extracted 3 times with ethyl acetate
  7. dry with materialthe combined organic phases dried (Na2SO4)
  8. customevaporated

출처 및 근거

ORD 기록
ord-46a497f317e24bad834bc37d5bbb63a2
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06900194B1

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