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

HRID 1494532노트

반응식

HRID 1494532 반응식
[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

참가 물질

6

반응물 3

HCID 313Hydrochloric Acid2회HCID 516892Sodium BicarbonateHCID 12821304N-(1-benzylpiperid-4-yl)-2-acetoxy-4-acetamido-5-nitrobenzamide

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매2회HCID 962Water용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-e216c34262aa47268c7c7f4d58680b76
출처 데이터셋
uspto-grants-1991_06
특허 번호
US05026858

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