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Hydrochloric Acid → 3,4-Dimethoxybicyclo[4.2.0]octa-1,3,5-trien-7-one

HRID 536999
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HRID 536999 반응식
C([O:3][C:4]1(OCC)[CH2:11][C:10]2[C:5]1=[CH:6][C:7]([O:14][CH3:15])=[C:8]([O:12][CH3:13])[CH:9]=2)C.Cl.O>C1COCC1.O>[CH3:13][O:12][C:8]1[CH:9]=[C:10]2[C:5](=[CH:6][C:7]=1[O:14][CH3:15])[C:4](=[O:3])[CH2:11]2
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 1176363657,7-Diethoxy-3,4-dimethoxybicyclo[4.2.0]octa-1,3,5-triene

생성물 1

HCID 27527583,4-Dimethoxybicyclo[4.2.0]octa-1,3,5-trien-7-one수율 81.2%

시약·촉매·용매 1

HCID 21881883Oxolane--water (1/1)용매

실험 절차

7,7-Diethoxy-3,4-dimethoxybicyclo[4.2.0]octa-1,3,5-triene (1.76 g, 6.98 mmol) is stirred in a mixture of THF/water (6/1) at ambient temperature. 815 mg of an aqueous 11N HCl solution (1.1 eq, 7.7 mmol) are then added. The reaction mixture is stirred for 2 hours ambient temperature. Water is added to facilitate two extractions with ethyl acetate (2×30 mL). The organic phases are dried over MgSO4 and then subjected to drying. There are obtained 1.01 g of the title product in the form of a grey powder.

후처리

  1. extractiontwo extractions with ethyl acetate (2×30 mL)
  2. dry with materialThe organic phases are dried over MgSO4
  3. customto drying

출처 및 근거

ORD 기록
ord-a55c9872dcac49f7952bb584fe88330a
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08859763B1

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