Valeronitrile → HCID 178446835, 화합물

HRID 1492188노트

반응식

HRID 1492188 반응식
Cl.[NH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:14][CH2:13][O:12][CH2:11][CH2:10]1.[C:15](#[N:20])[CH2:16][CH2:17][CH2:18][CH3:19].[OH-].[Na+]>>[O:12]1[CH2:13][CH2:14][N:9]([C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=2[NH:2][C:15](=[NH:20])[CH2:16][CH2:17][CH2:18][CH3:19])[CH2:10][CH2:11]1

참가 물질

4

반응물 3

HCID 8061ValeronitrileHCID 14798Sodium HydroxideHCID 189522842-Morpholinoaniline hydrochloride

생성물 1

HCID 178446835HCID 178446835, 화합물

실험 절차

A mixture of 4-(2-aminophenyl)morpholine hydrochloride (6.5 g) and valeronitrile (35 ml) were heated at 160°-165° C. under nitrogen for 25 hours and then cooled. The mixture was treated with aqueous sodium hydroxide and the basified mixture was extracted with dichloromethane. The solvent was removed by evaporation and the residue distilled under a pressure of 50 mm Hg to remove half the unreacted valeronitrile. A solid separated on cooling which was separated by filtration, washed with hexane (50 ml) and recrystallised from hexane to give N-(2-morpholinophenyl)valeramidine. (m.p. 135°-136° C.).

후처리

  1. temperaturewere heated at 160°-165° C. under nitrogen for 25 hours
  2. temperaturecooled
  3. extractionthe basified mixture was extracted with dichloromethane
  4. customThe solvent was removed by evaporation
  5. distillationthe residue distilled under a pressure of 50 mm Hg
  6. customto remove half the unreacted valeronitrile
  7. customA solid separated
  8. temperatureon cooling which
  9. customwas separated by filtration
  10. washwashed with hexane (50 ml)
  11. customrecrystallised from hexane

출처 및 근거

ORD 기록
ord-80a475de375f4b69b6e7998649002705
출처 데이터셋
uspto-grants-1994_12
특허 번호
US05373008

반응 노트

불러오는 중…