Sodium Bicarbonate → 1-(4-Chlorostyrene-beta-sulfonyl)-4-[4-methyl-2-(4-pyridyl)-5-thiazolecarbonyl]piperazine

HRID 278610ノート

反応式

HRID 278610 の反応式
Cl.Cl.[CH3:3][C:4]1[N:5]=[C:6]([C:17]2[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=2)[S:7][C:8]=1[C:9]([N:11]1[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]1)=[O:10].C(=O)(O)[O-].[Na+].[Cl:28][C:29]1[CH:40]=[CH:39][C:32]([CH:33]=[CH:34][S:35](Cl)(=[O:37])=[O:36])=[CH:31][CH:30]=1>C(OCC)(=O)C>[Cl:28][C:29]1[CH:30]=[CH:31][C:32]([CH:33]=[CH:34][S:35]([N:14]2[CH2:15][CH2:16][N:11]([C:9]([C:8]3[S:7][C:6]([C:17]4[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=4)=[N:5][C:4]=3[CH3:3])=[O:10])[CH2:12][CH2:13]2)(=[O:37])=[O:36])=[CH:39][CH:40]=1

参加物

5

反応物 3

HCID 516892Sodium BicarbonateHCID 38443052-(4-chlorophenyl)ethenesulfonyl ChlorideHCID 226280481-[4-Methyl-2-(4-pyridyl)-5-thiazolecarbonyl]piperazine dihydrochloride

生成物 1

HCID 570805581-(4-Chlorostyrene-beta-sulfonyl)-4-[4-methyl-2-(4-pyridyl)-5-thiazolecarbonyl]piperazine収率 62.4%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 1-[4-methyl-2-(4-pyridyl)-5-thiazolecarbonyl]piperazine dihydrochloride (200 mg) in ethyl acetate (10 ml)/sodium bicarbonate (10 ml) was added 4-chlorostyrene-β-sulfonylchloride (275 mg), and the mixture was stirred at room temperature for 1 hour. The ethyl acetate layer was separated, washed with brine, dried and concentrated. The residue was purified with silica gel column chromatography (ethyl acetate) to give colorless crystals of the title compound (169 mg).

後処理

  1. customThe ethyl acetate layer was separated
  2. washwashed with brine
  3. customdried
  4. concentrationconcentrated
  5. customThe residue was purified with silica gel column chromatography (ethyl acetate)

出典と根拠

ORDレコード
ord-9def6a6b956a47ec99152347c608f88d
出典データセット
uspto-grants-2002_03
特許番号
US06359134B1

反応ノート

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