Formic Acid → 2-Adamantanecarboxylic acid

HRID 1578417

反応式

HRID 1578417 の反応式
O[C:2]12[CH2:11][CH:6]3[CH2:7][CH:8]([CH2:10][CH:4]([CH2:5]3)[CH2:3]1)[CH2:9]2.OS(O)(=O)=O.[OH-].[Na+].[CH:19]([OH:21])=[O:20]>>[CH:2]12[CH2:11][CH:6]3[CH2:7][CH:8]([CH2:10][CH:4]([CH2:5]3)[CH:3]1[C:19]([OH:21])=[O:20])[CH2:9]2

参加物

5

反応物 4

HCID 284Formic AcidHCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 641521-Adamantanol

生成物 1

HCID 3038022-Adamantanecarboxylic acid

実験手順

hydroxyadamantane were dissolved in 30 mls of HCOOH 98-100 %, and this solution was added dropwise, while stirring vigorously, to 1.5 1. of H2SO4 96% cooled to 5°C. Stirring was then continued at the same temperature for 90 minutes and the mixture was finally poured out on ice. NaOH was added to the mixture until it has a pH of approximately 1 and the formed precipitate was extracted with diethyl ether. The extract was dried over Na2SO4 and the solvent was then evaporated. The cruse 2-adamantyl carboxylic acid was thus obtained, which was purified by two crystallizations from 70% ethanol. The purified acid had a melting point of 142-144°C.

後処理

  1. additionthis solution was added dropwise
  2. stirringStirring
  3. additionthe mixture was finally poured out on ice
  4. extractionthe formed precipitate was extracted with diethyl ether
  5. dry with materialThe extract was dried over Na2SO4
  6. customthe solvent was then evaporated

出典と根拠

ORDレコード
ord-122be41070054040ac94607a301cacf0
出典データセット
uspto-grants-1976_02
特許番号
US03936491

関連ノート

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