Methyl chloroformate → Ethyl 2-methoxycarbonyloxyimino-2-cyanoacetate

HRID 1283758

反応式

HRID 1283758 の反応式
[Na].[OH:2][N:3]=[C:4]([C:10]#[N:11])[C:5]([O:7][CH2:8][CH3:9])=[O:6].Cl[C:13]([O:15][CH3:16])=[O:14].C(=O)([O-])O.[Na+]>O.CC(C)=O>[CH3:16][O:15][C:13]([O:2][N:3]=[C:4]([C:10]#[N:11])[C:5]([O:7][CH2:8][CH3:9])=[O:6])=[O:14]

参加物

7

反応物 4

HCID 6586Methyl chloroformateHCID 516892Sodium BicarbonateHCID 5360545SodiumHCID 6399078Ethyl 2-cyano-2-(hydroxyimino)acetate

生成物 1

HCID 54529457Ethyl 2-methoxycarbonyloxyimino-2-cyanoacetate収率 82.2%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 962Water溶媒

実験手順

A solution of sodium salt of ethyl 2-hydroxyimino-2-cyanoacetate (41.0 g) in water (200 ml) is stirred under ice-cooling, and a solution of methyl chloroformate (23.6 g) in acetone (20 ml) is dropwise added thereto. The resulting mixture is adjusted to pH 6 to 7 with the addition of an aqueous solution of sodium hydrogencarbonate and stirred for 1 hour. The precipitates are collected by filtration, washed with water and dried to give ethyl 2-methoxycarbonyloxyimino-2-cyanoacetate (41.1 g) as crystals melting at 68° to 70°C which is identified with the compound obtained in Example 9 by IR absorption spectrum.

後処理

  1. temperaturecooling
  2. filtrationThe precipitates are collected by filtration
  3. washwashed with water
  4. customdried

出典と根拠

ORDレコード
ord-a6efa27fada64675bfa5c09f9ee5470a
出典データセット
uspto-grants-1976_08
特許番号
US03976635

関連ノート

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