Sulfuric Acid → 3-(1-Adamantyl)-4,5-methylenedioxybromobenzene

HRID 1078515

반응식

HRID 1078515 반응식
C(O[C:5]12[CH2:14][CH:9]3[CH2:10][CH:11]([CH2:13][CH:7]([CH2:8]3)[CH2:6]1)[CH2:12]2)(=O)C.S(=O)(=O)(O)O.[CH2:20]1[O:28][C:27]2[CH:26]=[CH:25][C:24]([Br:29])=[CH:23][C:22]=2[O:21]1.C(=O)(O)[O-].[Na+]>C1CCCCC1.CCCCCCC.O>[C:5]12([C:26]3[CH:25]=[C:24]([Br:29])[CH:23]=[C:22]4[O:21][CH2:20][O:28][C:27]=34)[CH2:6][CH:7]3[CH2:13][CH:11]([CH2:10][CH:9]([CH2:8]3)[CH2:14]1)[CH2:12]2

참가 물질

8

반응물 4

HCID 1118Sulfuric AcidHCID 758311-Bromo-3,4-(methylenedioxy)benzeneHCID 516892Sodium BicarbonateHCID 5199731-Adamantyl acetate

생성물 1

HCID 194297023-(1-Adamantyl)-4,5-methylenedioxybromobenzene

시약·촉매·용매 3

HCID 962Water용매HCID 8078Cyclohexane용매HCID 8900Heptane용매

실험 절차

4.82 g (24.9 mmol) of acetoxyadamantane and 0.75 ml (139 mmol) of concentrated sulphuric acid are added to 5 g (24.9 mmol) of 3,4-methylenedioxybromobenzene in 35 ml of cyclohexane and 35 ml of heptane. The reaction medium is stirred at room temperature overnight. This medium is then hydrolyzed with 250 ml of water, neutralized with sodium bicarbonate, extracted with 200 ml of dichloromethane, dried over magnesium sulphate and evaporated, to give 2.89 g (34.8%) of the expected derivative which melts at 134° C.)

후처리

  1. extractionextracted with 200 ml of dichloromethane
  2. dry with materialdried over magnesium sulphate
  3. customevaporated
  4. customto give 2.89 g (34.8%) of the expected derivative which melts at 134° C.)

출처 및 근거

ORD 기록
ord-c094ee2e80b94504a44171caaf46df4d
출처 데이터셋
uspto-grants-1996_08
특허 번호
US05547983

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