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

HRID 278610노트

반응식

HRID 278610 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-9def6a6b956a47ec99152347c608f88d
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06359134B1

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