Hydrochloric Acid → N-(1-benzylpiperid-4-yl)-2-hydroxy-4-amino-5-nitrobenzamide hydrochloride

HRID 1494532ノート

反応式

HRID 1494532 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([NH:14][C:15](=[O:33])[C:16]2[CH:21]=[C:20]([N+:22]([O-:24])=[O:23])[C:19]([NH:25]C(=O)C)=[CH:18][C:17]=2[O:29]C(=O)C)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[ClH:34].C(=O)(O)[O-].[Na+]>C(O)C.O>[ClH:34].[CH2:1]([N:8]1[CH2:9][CH2:10][CH:11]([NH:14][C:15](=[O:33])[C:16]2[CH:21]=[C:20]([N+:22]([O-:24])=[O:23])[C:19]([NH2:25])=[CH:18][C:17]=2[OH:29])[CH2:12][CH2:13]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 3

HCID 313Hydrochloric Acid2 回HCID 516892Sodium BicarbonateHCID 12821304N-(1-benzylpiperid-4-yl)-2-acetoxy-4-acetamido-5-nitrobenzamide

生成物 1

HCID 19828529N-(1-benzylpiperid-4-yl)-2-hydroxy-4-amino-5-nitrobenzamide hydrochloride

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回HCID 962Water溶媒2 回

実験手順

A suspension of N-(1-benzylpiperid-4-yl)-2-acetoxy-4-acetamido-5-nitrobenzamide (4.5 g; 0.01 mol) [prepared by the procedure described in Example 1] in ethanol (25 ml), concentrated hydrochloric acid (4.5 ml) and water (50 ml) was boiled under reflux for 2 hours. The mixture was diluted with water, made alkaline with sodium bicarbonate and extracted with chloroform. The organic solution was dried (Na2SO4), the solvent removed in vacuo and the residue triturated with diethyl ether to give a solid which was treated with a saturated solution of hydrogen chloride in ethanol. After crystallization from ethanol, 3 g of N-(1-benzylpiperid-4-yl)-2-hydroxy-4-amino-5-nitrobenzamide hydrochloride were obtained, m.p. 248°-250° C. (dec).

後処理

  1. customprepared by the procedure
  2. temperatureunder reflux for 2 hours
  3. extractionextracted with chloroform
  4. dry with materialThe organic solution was dried (Na2SO4)
  5. customthe solvent removed in vacuo
  6. customthe residue triturated with diethyl ether
  7. customto give a solid which
  8. customAfter crystallization from ethanol

出典と根拠

ORDレコード
ord-e216c34262aa47268c7c7f4d58680b76
出典データセット
uspto-grants-1991_06
特許番号
US05026858

反応ノート

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