Ethanol → Para-aminobenzylidenecamphor

HRID 2254510ノート

反応式

HRID 2254510 の反応式
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

参加物

6

反応物 3

HCID 702EthanolHCID 25517Ammonium ChlorideHCID 67855243Paranitrobenzylidenecamphor

生成物 1

HCID 68878284Para-aminobenzylidenecamphor収率 99%

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 962Water溶媒

実験手順

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:

後処理

  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

出典と根拠

ORDレコード
ord-bb1ad6f0bc584841b2b0836efcb78d68
出典データセット
uspto-grants-1993_08
特許番号
US05236698

反応ノート

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