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Triethylamine → N-(1-Benzylpiperid-4-yl)-2-methoxy-4-amino-5-nitrobenzamide

HRID 1494528
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HRID 1494528 반응식
[CH3:1][O:2][C:3]1[CH:11]=[C:10]([NH2:12])[C:9]([N+:13]([O-:15])=[O:14])=[CH:8][C:4]=1[C:5]([OH:7])=O.C(N(CC)CC)C.ClC(OCC)=O.[CH2:29]([N:36]1[CH2:41][CH2:40][CH:39]([NH2:42])[CH2:38][CH2:37]1)[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1>CN(C)C=O>[CH2:29]([N:36]1[CH2:41][CH2:40][CH:39]([NH:42][C:5](=[O:7])[C:4]2[CH:8]=[C:9]([N+:13]([O-:15])=[O:14])[C:10]([NH2:12])=[CH:11][C:3]=2[O:2][CH3:1])[CH2:38][CH2:37]1)[C:30]1[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=1
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참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 1010164-Amino-2-methoxy-5-nitrobenzoic acidHCID 4158521-Benzyl-4-piperidylamine

생성물 1

HCID 12821241N-(1-Benzylpiperid-4-yl)-2-methoxy-4-amino-5-nitrobenzamide수율 80.6%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매
4회

실험 절차

To a solution of 2-methoxy-4-amino-5-nitrobenzoic acid (6.4 g; 0.03 moles) in N,N-dimethylformamide (175 ml) a solution of triethylamine (3 g; 0.03 moles) in N,N-dimethylformamide (5 ml) was added. The mixture was cooled to -5° to -10° C. and a solution of ethyl chloroformate (3.3 g; 0.03 moles) in N,N-dimethylformamide (5 ml) was added. The reaction mixture was stirred at the same temperature for 0.5 hours and then a solution of 1-benzyl-4-aminopiperidine (5.7 g; 0.03 moles) in N,N-dimethylformamide (15 ml) was added. After stirring for 1 hour at -5° to -10° C., the temperature was allowed to reach room temperature overnight. The solvent was removed in vacuo and the residue was poured into an aqueous sodium bicarbonate solution. The resulting solid was exhaustively extracted with methylene chloride, the organic layers washed with an aqueous sodium bicarbonate solution and then with water, dried (Na2SO4 ) and the solvent removed in vacuo. N-(1-Benzylpiperid-4-yl)-2-methoxy-4-amino-5-nitrobenzamide (9.3 g) was obtained and converted into its hydrochloride by treatment with a saturated solution of ethanolic hydrogen chloride; the hydrochloride melted at 218°-220° C. (dec).

후처리

  1. temperatureThe mixture was cooled to -5° to -10° C.
  2. stirringAfter stirring for 1 hour at -5° to -10° C.
  3. waitto reach room temperature overnight
  4. customThe solvent was removed in vacuo
  5. additionthe residue was poured into an aqueous sodium bicarbonate solution
  6. extractionThe resulting solid was exhaustively extracted with methylene chloride
  7. washthe organic layers washed with an aqueous sodium bicarbonate solution
  8. dry with materialwith water, dried (Na2SO4 )
  9. customthe solvent removed in vacuo

출처 및 근거

ORD 기록
ord-847d97e38eaa42b69cd595e60757bcff
출처 데이터셋
uspto-grants-1991_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05026858

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