Potassium Carbonate → HCID 57708305、化合物

HRID 404819

反応式

HRID 404819 の反応式
Cl[C:2]1[N:7]=[CH:6][N:5]=[C:4]([NH:8][C:9]2[CH:10]=[C:11]([NH:15]C(=O)OC(C)(C)C)[CH:12]=[CH:13][CH:14]=2)[CH:3]=1.[Cl:23][C:24]1[CH:25]=[C:26]([OH:31])[CH:27]=[CH:28][C:29]=1[F:30].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C.O>[Cl:23][C:24]1[CH:25]=[C:26]([CH:27]=[CH:28][C:29]=1[F:30])[O:31][C:2]1[N:7]=[CH:6][N:5]=[C:4]([NH:8][C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([NH2:15])[CH:10]=2)[CH:3]=1

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 757903-Chloro-4-fluorophenolHCID 57708283HCID 57708283、化合物

生成物 1

HCID 57708305HCID 57708305、化合物収率 45.4%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A solution of tert-butyl 3-(6-chloropyrimidin-4-ylamino)phenylcarbamate (1.6 g, 5 mmol), 3-chloro-4-fluorophenol (1.4 g, 10 mmol) and potassium carbonate (1.4 g, 10 mmol) in 15 mL of DMF was heated to 120° C. for 16 h. The reaction mixture was mixed in 15 mL of water, the crude product was precipitated, filtered, purified by flash chromatography on silica gel with MeOH/DCM solvent system to afford 750 mg (45% yield) of N1-(6-(3-chloro-4-fluorophenoxy)pyrimidin-4-yl)benzene-1,3-diamine as an off-white solid. MS (m/z): MH+=331.

後処理

  1. customthe crude product was precipitated
  2. filtrationfiltered
  3. custompurified by flash chromatography on silica gel with MeOH/DCM solvent system

出典と根拠

ORDレコード
ord-3f19b32b16114826ac2328666cfec215
出典データセット
uspto-grants-2014_06
特許番号
US08748606B2

関連ノート

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