Methanesulfonyl chloride → HCID 59152218, 화합물

HRID 605592노트

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HRID 605592 반응식
[C:1]([N:5]1[C:9]([NH:10][C:11]2[N:16]=[C:15]([CH2:17]O)[CH:14]=[N:13][CH:12]=2)=[CH:8][CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2].C(N(C(C)C)CC)(C)C.CS([Cl:32])(=O)=O.[Cl-].[Li+]>C(Cl)(Cl)Cl.C(OCC)(=O)C.CN(C)C=O>[C:1]([N:5]1[C:9]([NH:10][C:11]2[CH:12]=[N:13][CH:14]=[C:15]([CH2:17][Cl:32])[N:16]=2)=[CH:8][CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2]

참가 물질

8

반응물 4

HCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 433294Lithium ChlorideHCID 59152207(6-((1-(tert-Butyl)-1H-pyrazol-5-yl)amino)pyrazin-2-yl)methanol

생성물 1

HCID 59152218HCID 59152218, 화합물

시약·촉매·용매 3

HCID 6212Chloroform용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 507.3 mg of (6-((1-tert-butyl-1H-pyrazol-5-yl)amino)pyrazin-2-yl)methanol in 6.8 ml of chloroform were successively added 1.08 ml of diisopropylethylamine and 0.24 ml of methylsulfonyl chloride under cooling with ice, followed by stirring the reaction mixture at room temperature for 1.5 hours. To the reaction mixture were successively added 442.9 mg of lithium chloride and 6.8 ml of N,N-dimethylformamide, followed by stirring the reaction mixture at room temperature for 2 hours. After diluting the reaction mixture with ethyl acetate, the ethyl acetate solution was successively washed with water and brine, dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated in vacuo. The resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate=20/1-1/4) to give the title compound as a yellow solid.

후처리

  1. temperatureunder cooling with ice
  2. stirringby stirring the reaction mixture at room temperature for 2 hours
  3. washthe ethyl acetate solution was successively washed with water and brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated in vacuo
  7. customThe resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate=20/1-1/4)

출처 및 근거

ORD 기록
ord-da4cc4201fb94fba85a51db0a598893b
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07915263B2

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