Methanesulfonyl chloride → HCID 59152218、化合物

HRID 605592ノート

反応式

HRID 605592 の反応式
[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]

参加物

8

反応物 4

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

生成物 1

HCID 59152218HCID 59152218、化合物

試薬・触媒・溶媒 3

HCID 6212Chloroform溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-da4cc4201fb94fba85a51db0a598893b
出典データセット
uspto-grants-2011_03
特許番号
US07915263B2

反応ノート

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