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Potassium Phosphate, Tribasic → 6-[[6-(Acetylamino)-pyrimidin-4-yl]oxy]-naphthalene-1-carboxylic acid [3-(4-methyl-imidazol-1-yl)-5-trifluoromethyl-phenyl]-amide

HRID 1512193
ノート
印刷プレビュー

反応式

HRID 1512193 の反応式
P([O-])([O-])([O-])=O.[K+].[K+].[K+].[OH:9][C:10]1[CH:11]=[C:12]2[C:17](=[CH:18][CH:19]=1)[C:16]([C:20]([NH:22][C:23]1[CH:28]=[C:27]([C:29]([F:32])([F:31])[F:30])[CH:26]=[C:25]([N:33]3[CH:37]=[C:36]([CH3:38])[N:35]=[CH:34]3)[CH:24]=1)=[O:21])=[CH:15][CH:14]=[CH:13]2.Cl[C:40]1[N:45]=[CH:44][N:43]=[C:42]([NH:46][C:47](=[O:49])[CH3:48])[CH:41]=1>C1(C)C=CC=CC=1>[CH3:38][C:36]1[N:35]=[CH:34][N:33]([C:25]2[CH:24]=[C:23]([NH:22][C:20]([C:16]3[C:17]4[C:12](=[CH:11][C:10]([O:9][C:40]5[CH:41]=[C:42]([NH:46][C:47](=[O:49])[CH3:48])[N:43]=[CH:44][N:45]=5)=[CH:19][CH:18]=4)[CH:13]=[CH:14][CH:15]=3)=[O:21])[CH:28]=[C:27]([C:29]([F:30])([F:31])[F:32])[CH:26]=2)[CH:37]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 62657Potassium Phosphate, TribasicHCID 539477N-(6-chloropyrimidin-4-yl)acetamideHCID 68591664HCID 68591664、化合物

生成物 1

HCID 251573116-[[6-(Acetylamino)-pyrimidin-4-yl]oxy]-naphthalene-1-carboxylic acid [3-(4-methyl-imidazol-1-yl)-5-trifluoromethyl-phenyl]-amide

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
110 °C

実験手順

Anhydrous tripotassium phosphate (848 mg, 4.0 mmol) is added to a stirred solution of 6-hydroxy-N-[3-(4-methyl-1H-imidazol-1-yl)-5-(trifluoromethyl)phenyl]-1-naphthalenecarboxamide (411 mg, 1.0 mmol) in toluene (40 mL) under an argon atmosphere at 110° C. N-(6-Chloro-4-pyrimidinyl)-acetamide (252 mg, 1.5 mmol) is added and the mixture is stirred at 110° C. for a further 50 hours. The solvent is evaporated off under reduced pressure and the residue is washed with a saturated aqueous solution of NH4Cl and dried. The crude product is purified by recrystallisation from methanol to afford the title compound as a beige solid, m.p.: 291-293° C.

後処理

  1. customThe solvent is evaporated off under reduced pressure
  2. washthe residue is washed with a saturated aqueous solution of NH4Cl
  3. customdried
  4. customThe crude product is purified by recrystallisation from methanol

出典と根拠

ORDレコード
ord-7f97b7ddad0041b4ba448616deaa80a4
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08217045B2

反応ノート

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