Triphenylphosphine → HCID 15512315、化合物

HRID 2258466

反応式

HRID 2258466 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[O:12][CH3:13])[N:8]([CH2:14][C:15]1[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[C:17]([O:23][CH3:24])[CH:16]=1)[N:7]=[C:6]2[CH2:25][C:26](O)=[O:27].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Cl:48][C:49]1[C:50]([CH3:61])=[C:51]([N:55]2[CH2:60][CH2:59][NH:58][CH2:57][CH2:56]2)[CH:52]=[CH:53][CH:54]=1>ClCCl>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[O:12][CH3:13])[N:8]([CH2:14][C:15]1[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[C:17]([O:23][CH3:24])[CH:16]=1)[N:7]=[C:6]2[CH2:25][C:26]([N:58]1[CH2:59][CH2:60][N:55]([C:51]2[CH:52]=[CH:53][CH:54]=[C:49]([Cl:48])[C:50]=2[CH3:61])[CH2:56][CH2:57]1)=[O:27]

参加物

5

反応物 3

HCID 11776TriphenylphosphineHCID 38008451-(3-Chloro-2-methylphenyl)piperazineHCID 15512314HCID 15512314、化合物

生成物 1

HCID 15512315HCID 15512315、化合物収率 100.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

実験手順

5,6-dimethoxy-1-(3,4-dimethoxybenzyl)-1H-indazole-3-acetic acid (41.0 g) was suspended in dichloromethane (500 ml). Then 2,2-dipyridyl disulfide (24.5 g) and triphenylphosphine (30.0 g) were added thereto and the mixture was stirred at room temperature. Next, (3-chloro-2-methyl-phenyl)piperazine (23.5 g) dissolved in dichloromethane (200 ml) was dropped thereinto within 5 minutes and the mixture was stirred at room temperature for 30 minutes. Then dichloromethane (1000 ml) was added to the reaction mixture. After washing with water, the organic layer was dried over sodium sulfate, filtered and evaporated under reduced pressure. The residue thus obtained was purified by using a silica gel column (ethyl acetate/hexane=2/1, silica gel 2 kg) to give 61.5 g of a colorless solid. This solid product was used in the subsequent reaction without purification. A small amount of this product was taken and recrystallized from ethanol. Thus colorless prism crystals (m.p.: 165°-169° C.) were obtained.

後処理

  1. additionwas dropped
  2. stirringthe mixture was stirred at room temperature for 30 minutes
  3. washAfter washing with water
  4. dry with materialthe organic layer was dried over sodium sulfate
  5. filtrationfiltered
  6. customevaporated under reduced pressure
  7. customThe residue thus obtained
  8. customwas purified

出典と根拠

ORDレコード
ord-538059eadcc740fbac56a5dc150e4d4c
出典データセット
uspto-grants-1997_08
特許番号
US05661150

関連ノート

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