4-Chlorobenzenesulfonyl chloride → HCID 9846568、化合物

HRID 1249719ノート

反応式

HRID 1249719 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8](Cl)(=[O:10])=[O:9])=[CH:4][CH:3]=1.Cl.Cl.Cl.[CH3:15][C:16]1[N:21]=[C:20]([N:22]2[CH2:27][CH2:26][N:25]([CH2:28][CH:29]3[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]3)[CH2:24][CH2:23]2)[CH:19]=[CH:18][N:17]=1.C(N(CC)CC)C>C(Cl)Cl>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:32]2[CH2:33][CH2:34][CH:29]([CH2:28][N:25]3[CH2:26][CH2:27][N:22]([C:20]4[CH:19]=[CH:18][N:17]=[C:16]([CH3:15])[N:21]=4)[CH2:23][CH2:24]3)[CH2:30][CH2:31]2)(=[O:10])=[O:9])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 73984-Chlorobenzenesulfonyl chlorideHCID 8471TriethylamineHCID 18328910HCID 18328910、化合物

生成物 1

HCID 9846568HCID 9846568、化合物収率 76.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

実験手順

A solution of 4-chlorophenylsulphonyl chloride (1.78 g) in methylene chloride (10 ml) was added dropwise over 15 minutes to a mixture of 4-[1-(2-methylpyrimidin-4-yl)piperazine-4-ylmethyl]piperidine trihydrochloride (2.78 g) and triethylamine (6.72 ml) in dichloromethane (40 ml) at 0° C. The solution was stirred at ambient temperature for 18 hours. The solution was diluted with dichloromethane and washed with water, dried (Na2SO4) and evaporated. The residue was purified by chromatography eluting with 4% methanol in dichloromethane. Recrystallisation from ethyl acetate/hexane gave, as a solid 1-(4-chlorophenylsulphonyl)-4-[1-(2-methylpyrimidin-4-yl)piperazin-4ylmethyl]piperidine (2.50 g), mp 191-193° C. (decomp.).

後処理

  1. washwashed with water
  2. dry with materialdried (Na2SO4)
  3. customevaporated
  4. customThe residue was purified by chromatography
  5. washeluting with 4% methanol in dichloromethane
  6. customRecrystallisation from ethyl acetate/hexane

出典と根拠

ORDレコード
ord-0b85241f0333445599018e83613de919
出典データセット
uspto-grants-2002_01
特許番号
US06335341B1

反応ノート

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