Hydrochloric Acid → HCID 20477659、化合物

HRID 2198511ノート

反応式

HRID 2198511 の反応式
C([O:3][C:4]([CH:6]1[C:8]([CH3:10])([CH3:9])[CH:7]1[C:11]#[N:12])=[O:5])C.[OH-].[K+].Cl>O.C(O)C>[C:11]([CH:7]1[C:8]([CH3:10])([CH3:9])[CH:6]1[C:4]([OH:5])=[O:3])#[N:12]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 128503382,2-Dimethyl-3-ethoxycarbonyl-cyclopropane-1-carbonitrile

生成物 1

HCID 20477659HCID 20477659、化合物収率 76.2%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

A suspension of 33.4 g (0.2 mol) of 2-cyano-3,3-dimethyl-cyclopropane-carboxylic acid ethyl ester and 16.8 g (0.3 mol) of potassium hydroxide in 200 ml of water and 100 ml of ethanol was stirred at 20°-25° C. for 15 hours. The alcohol was then stripped off and the aqueous solution was acidified with dilute hydrochloric acid and extracted twice with 100 ml of ether (or methylene chloride) each time. The combined organic extracts were dried over Na2SO4 and concentrated and the residue was distilled. 21.2 g (76% of theory) of 2-cyano-3,3-dimethyl-cyclopropane-carboxylic acid were obtained in the form of an oil of boiling point 110°-120° C., which crystallized on cooling (melting point: 101°-106° C.). ##STR44##

後処理

  1. extractionextracted twice with 100 ml of ether (or methylene chloride) each time
  2. dry with materialThe combined organic extracts were dried over Na2SO4
  3. concentrationconcentrated
  4. distillationthe residue was distilled

出典と根拠

ORDレコード
ord-dc88db577a54489bbbf7a08b2a456936
出典データセット
uspto-grants-1982_11
特許番号
US04358409

反応ノート

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