Hydrazine hydrate (1:1) → HCID 22011014, 화합물

HRID 323151노트

반응식

HRID 323151 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:9]([C:14]([NH:16][C:17]3[CH:49]=[CH:48][C:20]([C:21]([N:23]([CH3:47])[C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=4[O:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][N:36]4C(=O)C5=CC=CC=C5C4=O)=[O:22])=[CH:19][CH:18]=3)=[O:15])=[CH:10][CH:11]=[CH:12][CH:13]=2)=[CH:4][CH:3]=1.O.NN>C(O)C.C(OCC)C>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[C:9]([C:14]([NH:16][C:17]3[CH:18]=[CH:19][C:20]([C:21]([N:23]([CH3:47])[C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=4[O:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][NH2:36])=[O:22])=[CH:48][CH:49]=3)=[O:15])=[CH:10][CH:11]=[CH:12][CH:13]=2)=[CH:6][CH:7]=1

참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 22010690HCID 22010690, 화합물

생성물 1

HCID 22011014HCID 22011014, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 3283Diethyl Ether용매

실험 절차

A suspension of 4-(4′-methylbiphenyl-2-carboxamido)-N-methyl-N-[2-(5-phthalimidopentyloxy)phenyl]benzamide (1.1 g) in ethanol (20 ml) was stirred rapidly and treated with hydrazine hydrate (844 mg). The mixture was stirred at 60° C. for 3 hours. After cooling, the reaction mixture was diluted with diethyl ether and filtered through Celite. The Celite was washed with diethyl ether, and the filtrate was concentrated. The residual milky oil was again dissolved in diethyl ether, filtered through Celite, washed with diethyl ether, and concentrated to give 4-(4′-methylbiphenyl-2-carboxamido)-N-methyl-N-[2-(5-aminopentyloxy)phenyl]benzamide

후처리

  1. stirringThe mixture was stirred at 60° C. for 3 hours
  2. temperatureAfter cooling
  3. filtrationfiltered through Celite
  4. washThe Celite was washed with diethyl ether
  5. concentrationthe filtrate was concentrated
  6. dissolutionThe residual milky oil was again dissolved in diethyl ether
  7. filtrationfiltered through Celite
  8. washwashed with diethyl ether
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-49c9de55c9e049e1a499f8bc0666c42d
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06211242B1

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