Sulfuric Acid → HCID 18950694、化合物

HRID 1492552ノート

反応式

HRID 1492552 の反応式
O1CCOCC1.CO.C([NH:11][CH:12]([C:25]1[CH:26]=[N:27][CH:28]=[CH:29][CH:30]=1)[CH2:13][CH2:14][C:15]1[CH:24]=[CH:23][C:18]([C:19]([O:21][CH3:22])=[O:20])=[CH:17][CH:16]=1)=O.S(=O)(=O)(O)O.C(=O)([O-])O.[Na+]>>[NH2:11][CH:12]([C:25]1[CH:26]=[N:27][CH:28]=[CH:29][CH:30]=1)[CH2:13][CH2:14][C:15]1[CH:24]=[CH:23][C:18]([C:19]([O:21][CH3:22])=[O:20])=[CH:17][CH:16]=1

参加物

4

反応物 3

HCID 1118Sulfuric AcidHCID 516892Sodium BicarbonateHCID 86748334HCID 86748334、化合物

生成物 1

HCID 18950694HCID 18950694、化合物収率 87.4%

反応条件

温度
60 °C

実験手順

To 10 ml of the solution of 0.62 g of methyl 4-[3-formamido-3-(3-pyridyl)propyl]benzoate methanol-1,4 dioxane (1:1) was added 5 ml of 4% sulfuric acid, and stirred under heating at 60° C. overnight, which was then poured into saturated aqueous sodium hydrogencarbonate solution to be extracted with ethyl acetate. The obtained ethyl acetate phase was washed in saturated aqueous sodium chloride and dried over magnesium sulfate, to distill off the solvent, so that 0.35 g of methyl 4-[3-amino-3-(3-pyridyl)propyl]benzoate was yielded.

後処理

  1. extractionto be extracted with ethyl acetate
  2. washThe obtained ethyl acetate phase was washed in saturated aqueous sodium chloride
  3. dry with materialdried over magnesium sulfate
  4. distillationto distill off the solvent

出典と根拠

ORDレコード
ord-f3c8f0436cd3406f85d86598960cc551
出典データセット
uspto-grants-1994_12
特許番号
US05374641

反応ノート

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