p-Toluohydrazide → 4-Methyl-benzoic acid-(1-imino-ethyl)-hydrazide

HRID 29797ノート

反応式

HRID 29797 の反応式
[Na].Cl.[C:3](=[NH:8])(OCC)[CH3:4].[CH3:9][C:10]1[CH:19]=[CH:18][C:13]([C:14]([NH:16][NH2:17])=[O:15])=[CH:12][CH:11]=1>C(O)C>[NH:8]=[C:3]([N:16]([C:14](=[O:15])[C:13]1[CH:12]=[CH:11][C:10]([CH3:9])=[CH:19][CH:18]=1)[NH2:17])[CH3:4]

参加物

5

反応物 3

HCID 77174p-ToluohydrazideHCID 2724290Ethanimidic acid, ethyl ester, hydrochloride (1:1)HCID 5360545Sodium

生成物 1

HCID 684954674-Methyl-benzoic acid-(1-imino-ethyl)-hydrazide収率 15.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

1.65 g (72 mmol) sodium are dissolved in 80 mL ethanol. 8.89 g (72 mmol) ethyl acetimidate hydrochloride in 160 mL ethanol are added at ambient temperature and the precipitated sodium chloride is filtered off. The filtrate is combined with 6.00 g (40 mmol) 4-methyl-benzoic acid hydrazide and stirred overnight. The reaction mixture is evaporated down and cooled. The precipitated solid is filtered off and washed with cold ethanol and diethyl ether (5.7 g white solid). A further 1.2 g solid are obtained from the filtrate after distillation of the solvents and recrystallisation from ethanol.

後処理

  1. filtrationthe precipitated sodium chloride is filtered off
  2. customThe reaction mixture is evaporated down
  3. temperaturecooled
  4. filtrationThe precipitated solid is filtered off
  5. washwashed with cold ethanol and diethyl ether (5.7 g white solid)

出典と根拠

ORDレコード
ord-7072e1c97cbd4655b956b63c85fe56c9
出典データセット
uspto-grants-2008_09
特許番号
US07423036B2

反応ノート

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