Cornforth reagent → (2,4-Dichloro-6-(2-(isopropylsulfonyl)phenylamino)pyrimidin-5-yl)(phenyl)methanone

HRID 2046986ノート

反応式

HRID 2046986 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([Cl:8])[C:5]([CH:9]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[OH:10])=[C:4]([NH:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=2[S:24]([CH:27]([CH3:29])[CH3:28])(=[O:26])=[O:25])[N:3]=1.C1C=C[NH+]=CC=1.C1C=C[NH+]=CC=1.[O-][Cr](O[Cr]([O-])(=O)=O)(=O)=O>C(Cl)Cl>[Cl:1][C:2]1[N:7]=[C:6]([Cl:8])[C:5]([C:9]([C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=2)=[O:10])=[C:4]([NH:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=2[S:24]([CH:27]([CH3:29])[CH3:28])(=[O:26])=[O:25])[N:3]=1

参加物

4

反応物 2

HCID 2724130Cornforth reagentHCID 58290857(2,4-Dichloro-6-(2-(isopropylsulfonyl)phenylamino)pyrimidin-5-yl)(phenyl)methanol

生成物 1

HCID 58290891(2,4-Dichloro-6-(2-(isopropylsulfonyl)phenylamino)pyrimidin-5-yl)(phenyl)methanone

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To the solution of (2,4-dichloro-6-(2-(isopropylsulfonyl)phenylamino)pyrimidin-5-yl)(phenyl)methanol (113.4 mg, 0.25 mmol) in DCM (10 mL) was added PDC (236 mg, 0.63 mmol). The reaction mixture was stirred at room temperature overnight. The resulting mixture was then filtered through a pad of silica gel, and the pad was washed by 5% EtOAc in DCM (200 mL). The filtrate was concentrated in vacuo to afford (2,4-dichloro-6-(2-(isopropylsulfonyl)phenylamino)pyrimidin-5-yl)(phenyl)methanone as a colorless oil. MS (ES+): 450.0 (MH+).

後処理

  1. filtrationThe resulting mixture was then filtered through a pad of silica gel
  2. washthe pad was washed by 5% EtOAc in DCM (200 mL)
  3. concentrationThe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-ab2b4bd584b34282a82a3e058ffa7bcc
出典データセット
uspto-grants-2013_11
特許番号
US08592432B2

反応ノート

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