Ethanol → Para-aminobenzylidenecamphor

HRID 2254510노트

반응식

HRID 2254510 반응식
C(O)C.[Cl-].[NH4+].[N+:6]([C:9]1[CH:26]=[CH:25][C:12]([CH:13]=[C:14]2[CH:19]3[C:20]([CH3:22])([CH3:21])[C:16]([CH3:23])([CH2:17][CH2:18]3)[C:15]2=[O:24])=[CH:11][CH:10]=1)([O-])=O>[Zn].O>[NH2:6][C:9]1[CH:10]=[CH:11][C:12]([CH:13]=[C:14]2[CH:19]3[C:20]([CH3:22])([CH3:21])[C:16]([CH3:23])([CH2:17][CH2:18]3)[C:15]2=[O:24])=[CH:25][CH:26]=1

참가 물질

6

반응물 3

HCID 702EthanolHCID 25517Ammonium ChlorideHCID 67855243Paranitrobenzylidenecamphor

생성물 1

HCID 68878284Para-aminobenzylidenecamphor수율 99%

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 962Water용매

실험 절차

A mixture of fine zinc powder (60 g), ethanol (250 ml), ammonium chloride (2 g) and water (20 ml) is heated to the reflux temperature and the paranitrobenzylidenecamphor (20 g, 0.07 mol) is added in portions with stirring. The mixture is allowed to reflux for half an hour, the zinc is filtered and the mixture is rinsed with alcohol. The filtrate is poured in ice (500 g). The precipitate obtained is filtered, washed with water and dried under vacuum. A quantitative yield of para-aminobenzylidenecamphor (17.7 g) is obtained. It is recrystallised in ethanol to give the expected derivative:

후처리

  1. temperatureis heated to the reflux temperature
  2. temperatureto reflux for half an hour
  3. filtrationthe zinc is filtered
  4. washthe mixture is rinsed with alcohol
  5. additionThe filtrate is poured in ice (500 g)
  6. customThe precipitate obtained
  7. filtrationis filtered
  8. washwashed with water
  9. customdried under vacuum

출처 및 근거

ORD 기록
ord-bb1ad6f0bc584841b2b0836efcb78d68
출처 데이터셋
uspto-grants-1993_08
특허 번호
US05236698

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