Potassium Hydroxide → HCID 12850336、化合物

HRID 544090ノート

反応式

HRID 544090 の反応式
[CH3:1][C:2]1([CH3:17])[CH:4]([C:5]([O:7][CH2:8][CH3:9])=[O:6])[C:3]1([C:15]#[N:16])[C:10]([O:12]CC)=[O:11].[OH-].[K+]>>[CH3:17][C:2]1([CH3:1])[CH:4]([C:5]([O:7][CH2:8][CH3:9])=[O:6])[C:3]1([C:15]#[N:16])[C:10]([OH:12])=[O:11]

参加物

3

反応物 2

HCID 14797Potassium HydroxideHCID 12850335Ethyl 2,2-dimethyl-3-ethoxycarbonyl-1-cyano-cyclopropane-1-carboxylate

生成物 1

HCID 12850336HCID 12850336、化合物収率 90.6%

実験手順

A mixture of 2 g of ethyl 2,2-dimethyl-3-ethoxycarbonyl-1-cyano-cyclopropane-1-carboxylate (prepared as in U.S. Pat. No. 3,397,223) and 4.71 g of 10% ethanolic potassium hydroxide was stirred under an inert atmosphere for 15 hours and the ethanol was then evaporated under reduced pressure. The residue was washed with ether and was then taken up in ether. The pH of the solution was adjusted to 3 by addition of dilute sulfuric acid and the decanted ether phase was washed with water, dried and evaporated to dryness under reduced pressure to obtain 1.6 g of 2,2-dimethyl-3-ethoxycarbonyl-1-cyano-cyclopropane-1-carboxylic acid with a melting point of ≃130° C. (decomposition).

後処理

  1. customprepared as in U.S
  2. customthe ethanol was then evaporated under reduced pressure
  3. washThe residue was washed with ether
  4. additionThe pH of the solution was adjusted to 3 by addition of dilute sulfuric acid
  5. washthe decanted ether phase was washed with water
  6. customdried
  7. customevaporated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-2b48633f368f4cb4a30b8681ac8b6ae2
出典データセット
uspto-grants-1984_05
特許番号
US04448728

反応ノート

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