Methanol → HCID 14127257, 화합물

HRID 648667노트

반응식

HRID 648667 반응식
Cl[C:2]1(Cl)[CH:9]2[CH:4]([CH2:5][CH2:6][CH:7]=[CH:8]2)[C:3]1=[O:10].C(N(CC)CC)C.[Cl-].[NH4+].[CH3:21][OH:22]>[Cu].[Zn]>[CH3:21][O:22][C:4]12[C:3](=[O:10])[CH2:2][CH:9]1[CH:8]=[CH:7][CH2:6][CH2:5]2

참가 물질

6

반응물 4

HCID 887MethanolHCID 8471TriethylamineHCID 25517Ammonium ChlorideHCID 125073478,8-Dichlorobicyclo[4.2.0]oct-2-en-7-one

생성물 1

HCID 14127257HCID 14127257, 화합물

시약·촉매·용매 1

HCID 10290809Zinc copper couple촉매

실험 절차

To a stirred solution of 60 g of 8,8-dichlorobicyclo[4.2.0]oct-2-en-7-one in 500 ml of methanol under nitrogen at room temperature was added 48 ml of triethylamine over a period of 1 hour. The mixture was stirred for 30 minutes, then 90 g of ammonium chloride and 60 g of zinc-copper couple (as a powder) was added. The reaction mixture was stirred at room temperature for 2.5 hours, filtered through celite and the solvent removed under reduced pressure. The residue was dissolved in ethyl acetate, washed with brine, dried over anhydrous sodium sulfate and the solvent was distilled under vacuum, giving 32 g of 6-methoxybicyclo[4.2.0]oct-2-en-7-one.

후처리

  1. stirringThe reaction mixture was stirred at room temperature for 2.5 hours
  2. filtrationfiltered through celite
  3. customthe solvent removed under reduced pressure
  4. dissolutionThe residue was dissolved in ethyl acetate
  5. washwashed with brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationthe solvent was distilled under vacuum

출처 및 근거

ORD 기록
ord-68d29e0a70ed4194a2848ea4e9bfa160
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04735966

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