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Thionyl Chloride → N-{4-[(6,7-Dimethoxy-4-quinolyl)oxy]phenyl}-N'-[4-(morpholinomethyl)benzoyl]thiourea

HRID 721928
ノート
印刷プレビュー

反応式

HRID 721928 の反応式
S(Cl)(Cl)=O.O1CCN(CC2C=CC(C(Cl)=O)=CC=2)CC1.[CH3:21][O:22][C:23]1[CH:24]=[C:25]2[C:30](=[CH:31][C:32]=1[O:33][CH3:34])[N:29]=[CH:28][CH:27]=[C:26]2[O:35][C:36]1[CH:42]=[CH:41][C:39]([NH2:40])=[CH:38][CH:37]=1.[O:43]1[CH2:48][CH2:47][N:46]([CH2:49][C:50]2[CH:55]=[CH:54][C:53]([C:56]([N:58]=[C:59]=[S:60])=[O:57])=[CH:52][CH:51]=2)[CH2:45][CH2:44]1>C1(C)C=CC=CC=1.C(O)C>[CH3:21][O:22][C:23]1[CH:24]=[C:25]2[C:30](=[CH:31][C:32]=1[O:33][CH3:34])[N:29]=[CH:28][CH:27]=[C:26]2[O:35][C:36]1[CH:42]=[CH:41][C:39]([NH:40][C:59]([NH:58][C:56](=[O:57])[C:53]2[CH:52]=[CH:51][C:50]([CH2:49][N:46]3[CH2:45][CH2:44][O:43][CH2:48][CH2:47]3)=[CH:55][CH:54]=2)=[S:60])=[CH:38][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

7

反応物 4

HCID 24386Thionyl ChlorideHCID 115945434-[(6,7-Dimethoxyquinolin-4-yl)oxy]anilineHCID 137489614-Morpholin-4-ylmethyl-benzoyl chlorideHCID 21891082HCID 21891082、化合物

生成物 1

HCID 21890489N-{4-[(6,7-Dimethoxy-4-quinolyl)oxy]phenyl}-N'-[4-(morpholinomethyl)benzoyl]thiourea収率 78%

試薬・触媒・溶媒 2

HCID 702
Ethanol
溶媒
2 回
HCID 1140Toluene溶媒2 回

反応条件

温度
100 °C

実験手順

Commercially available 4-bromomethylbenzoic acid (300 mg) was dissolved in acetonitrile (10 ml). Potassium carbonate (30 mg) and morpholine (130 μl) were added to the solution, and the mixture was stirred at room temperature for one hr. The reaction layer was subjected to separation with chloroform and a saturated aqueous sodium hydrogencarbonate solution. The organic layer was then concentrated to give methyl 4-(morpholinomethyl)benzoate. Methanol (1 ml), water (150 μl), and potassium hydroxide (15 mg) were added to the residue, and the mixture was heated at 60° C. for one hr. After the completion of the reaction, the solvent was removed by distillation to give 4-(morpholinomethyl)benzoic acid. Toluene (20 ml) and thionyl chloride (1 ml) were added to the residule, and the mixture was heated at 100° C. for one hr. The solvent was removed by distillation, and 4-(morpholinomethyl)-1-benzenecarbonyl isothiocyanate was prepared using the resultant 4-(morpholinomethyl)-1-benzenecarbonyl chloride as a starting compound according to the description of the literature. 4-[(6,7-Dimethoxy-4-quinolyl)oxy]aniline (50 mg) was dissolved in toluene (5 ml) and ethanol (1 ml) to prepare a solution. A solution of 4-(morpholinomethyl)-1-benzenecarbonyl isothiocyanate in ethanol (1 ml) was then added to the solution, and the mixture was stirred at room temperature for 2 hr. The reaction solution was concentrated, and the residue was purified by chromatography on silica gel using chloroform/acetone for development to give the title compound (74 mg, yield 78%).

後処理

  1. customThe solvent was removed by distillation, and 4-(morpholinomethyl)-1-benzenecarbonyl isothiocyanate
  2. customwas prepared
  3. concentrationThe reaction solution was concentrated
  4. customthe residue was purified by chromatography on silica gel

出典と根拠

ORDレコード
ord-ab4aa044499a4e59900bf455812a04e1
出典データセット
uspto-grants-2006_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07135466B2

反応ノート

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