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Triethylamine → 3-Methyl-1-(2-naphthylsulphonyl)-4-[1-(4-pyridyl)piperidin-4-ylcarbonyl]piperazine

HRID 2288715
ノート
印刷プレビュー

反応式

HRID 2288715 の反応式
[CH3:1][CH:2]1[NH:7][CH2:6][CH2:5][N:4]([S:8]([C:11]2[CH:20]=[CH:19][C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[CH:12]=2)(=[O:10])=[O:9])[CH2:3]1.C(N(CC)CC)C.[N:28]1[CH:33]=[CH:32][C:31]([N:34]2[CH2:39][CH2:38][CH:37]([C:40](Cl)=[O:41])[CH2:36][CH2:35]2)=[CH:30][CH:29]=1>C(Cl)Cl>[CH3:1][CH:2]1[N:7]([C:40]([CH:37]2[CH2:36][CH2:35][N:34]([C:31]3[CH:30]=[CH:29][N:28]=[CH:33][CH:32]=3)[CH2:39][CH2:38]2)=[O:41])[CH2:6][CH2:5][N:4]([S:8]([C:11]2[CH:20]=[CH:19][C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[CH:12]=2)(=[O:10])=[O:9])[CH2:3]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 111837001-(4-Pyridinyl)-4-piperidinecarbonyl chlorideHCID 227219393-Methyl-1-(2-naphthylsulphonyl)piperazine

生成物 1

HCID 219999783-Methyl-1-(2-naphthylsulphonyl)-4-[1-(4-pyridyl)piperidin-4-ylcarbonyl]piperazine収率 32%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

3-Methyl-1-(2-naphthylsulphonyl)piperazine (1.8 g) and triethylamine (3.18 ml) were added in turn to a stirred solution of 1-(4-pyridyl)piperidine-4-carbonyl chloride (1.54 g) in methylene chloride (20 ml) and the mixture was stirred at ambient temperature for 16 hours. The mixture was partitioned between ethyl acetate and water. The organic phase was washed with water, dried (MgSO4) and evaporated. The residue was purified by column chromatography using a 89:10:1 mixture of ethyl acetate; methanol and ammonia as eluent. The material so obtained was triturated under diethyl ether to give 3-methyl-1-(2-naphthylsulphonyl)-4-[1-(4-pyridyl)piperidin-4-yl-carbonyl]piperazine (32% yield);

後処理

  1. customThe mixture was partitioned between ethyl acetate and water
  2. washThe organic phase was washed with water
  3. dry with materialdried (MgSO4)
  4. customevaporated
  5. customThe residue was purified by column chromatography
  6. additiona 89:10:1 mixture of ethyl acetate
  7. customThe material so obtained
  8. customwas triturated under diethyl ether

出典と根拠

ORDレコード
ord-b1258c1814704f8ea597b464eeb0079f
出典データセット
uspto-grants-2000_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06090813

反応ノート

読み込み中…

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