Ethyl cyanoacetate → HCID 178507928, 화합물

HRID 597502

반응식

HRID 597502 반응식
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

참가 물질

3

반응물 2

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

생성물 1

HCID 178507928HCID 178507928, 화합물

실험 절차

The appropriate aniline p-toluenesulfonate and ethyl cyanoacetate are combined in equimolar quantities and heated at 225° to 260° C. until a melt resulted. (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 one 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 one 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.

후처리

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

출처 및 근거

ORD 기록
ord-c41154695f164f138fff195b6dfe4258
출처 데이터셋
uspto-grants-1977_03
특허 번호
US04014881

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