Ethyl cyanoacetate → HCID 178507928、化合物

HRID 437539ノート

反応式

HRID 437539 の反応式
C1(C)C=CC(S(O)(=O)=O)=CC=1.[NH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.[C:19]([CH2:21][C:22](OCC)=[O:23])#[N:20]>>[NH2:20][C:19]1[CH:21]=[C:22]([OH:23])[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[N:12]=1

参加物

3

反応物 2

HCID 7764Ethyl cyanoacetateHCID 84165Benzenamine, 4-methylbenzenesulfonate (1:1)

生成物 1

HCID 178507928HCID 178507928、化合物

実験手順

The appropriate aniline p-toluenesulfonate and ethyl cyanoacetate are combined in equimolar quantities and heated at 225° to 260° C. until a melt required. (Higher temperatures are used if necessary to achieve a melt). The temperature of the melt is lowered to 240° to 250° C. and heating continued for 1 hour. The hot melt is poured into ice-cold chloroform (about 1 to 1.5 liters per mole of aniline reactant) and the mixture stirred for 1 hour. The solid is filtered off, added to water-ethanol (1 liter of 1:1 per mole of aniline reactant) at 45° to 50° C. and the solution made basic with ammonium hydroxide. The solid is separated by filtration and recrystallized from a suitable solvent such as isopropanol.

後処理

  1. temperatureheated at 225° to 260° C. until a melt
  2. customis lowered to 240° to 250° C.
  3. temperatureheating
  4. additionThe hot melt is poured into ice-cold chloroform (about 1 to 1.5 liters per mole of aniline reactant)
  5. filtrationThe solid is filtered off
  6. additionadded to water-ethanol (1 liter of 1:1 per mole of aniline reactant) at 45° to 50° C.
  7. customThe solid is separated by filtration
  8. customrecrystallized from a suitable solvent such as isopropanol

出典と根拠

ORDレコード
ord-16b1288da846456487d781eef8eca753
出典データセット
uspto-grants-1977_06
特許番号
US04031217

反応ノート

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