Hydrazine hydrate (1:1) → HCID 22011014、化合物

HRID 323151ノート

反応式

HRID 323151 の反応式
[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

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 22010690HCID 22010690、化合物

生成物 1

HCID 22011014HCID 22011014、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 3283Diethyl Ether溶媒

実験手順

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

後処理

  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

出典と根拠

ORDレコード
ord-49c9de55c9e049e1a499f8bc0666c42d
出典データセット
uspto-grants-2001_04
特許番号
US06211242B1

反応ノート

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