HCID 53929412, 화합물 → Ethyl (+/-)-4-trichloromethyl-6,6-dimethyl-2-oxo-3-oxabicyclo-[3.1.0]hexane-1-carboxylate

HRID 127037

반응식

HRID 127037 반응식
[N+](=[C:3]([C:9]([O:11][CH:12]([C:17]([Cl:20])([Cl:19])[Cl:18])[CH:13]=[C:14]([CH3:16])[CH3:15])=[O:10])[C:4]([O:6][CH2:7][CH3:8])=[O:5])=[N-]>CCCCCCCC.[Cu]>[Cl:18][C:17]([Cl:20])([Cl:19])[CH:12]1[CH:13]2[C:3]([C:4]([O:6][CH2:7][CH3:8])=[O:5])([C:14]2([CH3:16])[CH3:15])[C:9](=[O:10])[O:11]1

참가 물질

4

반응물 1

HCID 53929412HCID 53929412, 화합물

생성물 1

HCID 12525249Ethyl (+/-)-4-trichloromethyl-6,6-dimethyl-2-oxo-3-oxabicyclo-[3.1.0]hexane-1-carboxylate

시약·촉매·용매 2

HCID 23978Copper촉매HCID 356Octane용매2회

실험 절차

To a refluxing suspension of copper powder (5.0 g, 0.079 mole) in 240 ml of n-octane was added dropwise in one hour a solution of ethyl (±)-3-methyl-1-trichloromethyl-2-butenyl diazomalonate (5.0 g, 0.0146 mole) in 60 ml of n-octane. The reaction mixture was then heated under reflux for 21/2 hours and filtered. The n-octane was removed from the filtrate by evaporation under vacuum, yielding a residue which was distilled under vacuum to give ethyl (±)-4-trichloromethyl-6,6-dimethyl-2-oxo-3-oxabicyclo-[3.1.0]hexane-1-carboxylate as a highly viscous oil (2.47 g, 54% yield); bp, 123°-125°/0.3 mm.

후처리

  1. temperatureThe reaction mixture was then heated
  2. temperatureunder reflux for 21/2 hours
  3. filtrationfiltered
  4. customThe n-octane was removed from the filtrate by evaporation under vacuum
  5. customyielding a residue which
  6. distillationwas distilled under vacuum

출처 및 근거

ORD 기록
ord-ccd1b7912f6b421a96814214cccc1cee
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04254282

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