Potassium Carbonate → HCID 22508909、化合物

HRID 1163055ノート

反応式

HRID 1163055 の反応式
[F:1][C:2]1[C:10]([O:11][C:12]2[C:17]3=[C:18]([CH3:26])[C:19]([O:21][CH2:22][CH:23]4[CH2:25][O:24]4)=[CH:20][N:16]3[N:15]=[CH:14][N:13]=2)=[CH:9][CH:8]=[C:7]2[C:3]=1[CH:4]=[C:5]([CH3:27])[NH:6]2.[CH3:28][N:29]([CH3:34])[S:30]([NH2:33])(=[O:32])=[O:31].[C:35](=O)([O-])[O-].[K+].[K+]>CN(C=O)C.ClCCl>[F:1][C:2]1[C:10]([O:11][C:12]2[C:17]3=[C:18]([CH3:26])[C:19]([O:21][CH2:22][CH:23]([OH:24])[CH2:25][CH2:35][NH:33][S:30]([N:29]([CH3:34])[CH3:28])(=[O:32])=[O:31])=[CH:20][N:16]3[N:15]=[CH:14][N:13]=2)=[CH:9][CH:8]=[C:7]2[C:3]=1[CH:4]=[C:5]([CH3:27])[NH:6]2

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 134472N,N-DimethylsulfamideHCID 22508879HCID 22508879、化合物

生成物 1

HCID 22508909HCID 22508909、化合物収率 25%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

実験手順

A mixture of Example 2 (40 mg, 0.11 mmol), N,N-dimethylsulfamide (94 mg, 0.66 mmol) and potassium carbonate (91 mg, 0.66 mmol) in DMF (0.5 ml) was stirred at 80° C. for 1.5 h. The mixture was diluted with dichloromethane, filtered and concentrated in vacuo. The crude material was purified by preparative HPLC, followed by chromatography on silica gel eluting with 10% methanol in ethyl acetate to afford the title compound (13.7 mg, 25% yield) as a white solid. MS: (M+H)+=493.1

後処理

  1. filtrationfiltered
  2. concentrationconcentrated in vacuo
  3. customThe crude material was purified by preparative HPLC

出典と根拠

ORDレコード
ord-f0be806b552548c2a1945fc6406bfa88
出典データセット
uspto-grants-2010_10
特許番号
US07820814B2

反応ノート

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