Water → N-(3-Methylsulfonylphenyl)-N'-(4-(6-phenylaminopyrimidin-4-yloxy)phenyl)urea

HRID 853519ノート

反応式

HRID 853519 の反応式
[NH2:1][C:2]1[CH:21]=[CH:20][C:5]([O:6][C:7]2[N:12]=[CH:11][N:10]=[C:9]([NH:13][C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[CH:8]=2)=[CH:4][CH:3]=1.C1([O:28][C:29](=O)[NH:30][C:31]2[CH:36]=[CH:35][CH:34]=[C:33]([S:37]([CH3:40])(=[O:39])=[O:38])[CH:32]=2)C=CC=CC=1.O>CS(C)=O.C(OCC)(=O)C.CCCCCC>[CH3:40][S:37]([C:33]1[CH:32]=[C:31]([NH:30][C:29]([NH:1][C:2]2[CH:21]=[CH:20][C:5]([O:6][C:7]3[CH:8]=[C:9]([NH:13][C:14]4[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=4)[N:10]=[CH:11][N:12]=3)=[CH:4][CH:3]=2)=[O:28])[CH:36]=[CH:35][CH:34]=1)(=[O:38])=[O:39]

参加物

7

反応物 3

HCID 962WaterHCID 22936234Phenyl 3-methylsulfonylphenylcarbamateHCID 22936405N-(6-(4-Aminophenoxy)pyrimidin-4-yl)phenylamine

生成物 1

HCID 22936246N-(3-Methylsulfonylphenyl)-N'-(4-(6-phenylaminopyrimidin-4-yloxy)phenyl)urea収率 81%

試薬・触媒・溶媒 3

HCID 679Dimethyl Sulfoxide溶媒HCID 8058Hexane溶媒HCID 8857Ethyl Acetate溶媒2 回

実験手順

N-(6-(4-Aminophenoxy)pyrimidin-4-yl)phenylamine (55.6 mg, 0.200 mmol) and (3-methylsulfonylphenyl)carbamic acid phenyl ester (63.8 mg, 0.220 mmol) were heated and stirred in dimethylsulfoxide (1 ml) at 85° C. for 2 hours. The reaction solution was distributed between ethyl acetate and water, the organic layer was washed with 1N aqueous sodium hydroxide, water and saturated brine and dried over anhydrous magnesium sulfate, the drying agent was filtered off and the filtrate was distilled off under reduced pressure. The obtained crude product was suspended in ethyl acetate, the suspension was diluted with hexane, and the crystals were filtered out, washed with hexane and then blow-dried to obtain the title compound (77.0 mg, 0.162 mmol, 81%) as colorless crystals.

後処理

  1. washthe organic layer was washed with 1N aqueous sodium hydroxide, water and saturated brine
  2. dry with materialdried over anhydrous magnesium sulfate
  3. filtrationthe drying agent was filtered off
  4. distillationthe filtrate was distilled off under reduced pressure
  5. customThe obtained crude product
  6. filtrationthe crystals were filtered out
  7. washwashed with hexane
  8. customblow-dried

出典と根拠

ORDレコード
ord-619f10f97a754401a5a6add406c21531
出典データセット
uspto-grants-2007_08
特許番号
US07253286B2

反応ノート

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