Water → HCID 13086534、化合物

HRID 2416984ノート

反応式

HRID 2416984 の反応式
[CH3:1][C:2]12[CH2:11][CH:6]3[CH2:7][CH:8]([CH2:10][C:4]([OH:12])([CH2:5]3)[CH2:3]1)[CH2:9]2.[C:13](OC(=O)C)(=[O:15])[CH3:14].S(=O)(=O)(O)O.O.C(=O)(O)[O-].[Na+]>CCCCCCC.C1CCCCC1.CCOCC>[C:13]([O:12][C:4]12[CH2:5][CH:6]3[CH2:7][CH:8]([CH2:9][C:2]([CH3:1])([CH2:11]3)[CH2:3]1)[CH2:10]2)(=[O:15])[CH3:14]

参加物

9

反応物 5

HCID 962WaterHCID 1118Sulfuric AcidHCID 7918Acetic AnhydrideHCID 516892Sodium BicarbonateHCID 40715573-Methyl-1-adamantanol

生成物 1

HCID 13086534HCID 13086534、化合物

試薬・触媒・溶媒 3

HCID 3283Diethyl Ether溶媒HCID 8078Cyclohexane溶媒HCID 8900Heptane溶媒

実験手順

121 mg (0.728 mmoles) of 3-methyl-1-adamantanol are dissolved in 0.2 mL n-heptane and 0.2 mL cyclohexane. A mixture of 0.2 mL (2.25 mmoles) of acetic anhydride and 2 microliters (0.036 mmoles) of concentrated sulfuric acid is added, and the mixture is at ambient temperature for 20.5 hours. The solution is dissolved in 10 L of ether and extracted with 10 mL of water. The aqueous layer is extracted with 10 mL ether. The ether layers are combined, extracted with 2×mL of water followed by 40 mL of aqueous sodium bicarbonate (10 g/liter), dried over magnesium sulfate, and stripped of solvent in vacuo. The product is a colorless oil with Rf 0.55 (silica: eluant hexane 75%, ethyl acetate 25%).

後処理

  1. additionis added
  2. extractionextracted with 10 mL of water
  3. extractionThe aqueous layer is extracted with 10 mL ether
  4. dry with materialdried over magnesium sulfate

出典と根拠

ORDレコード
ord-23dee9fbdebb4e60a3d63ced5fa5ffbe
出典データセット
uspto-grants-2004_11
特許番号
US06825226B2

反応ノート

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