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

HRID 1078515

反応式

HRID 1078515 の反応式
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

参加物

8

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 8078Cyclohexane溶媒HCID 8900Heptane溶媒

実験手順

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.)

後処理

  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.)

出典と根拠

ORDレコード
ord-c094ee2e80b94504a44171caaf46df4d
出典データセット
uspto-grants-1996_08
特許番号
US05547983

関連ノート

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