Hydrochloric Acid → N-[6-chloro-5-(2-methoxyphenoxy)-2-(2-pyrimidinyl)-4-pyrimidinyl]-2-phenylethenesulfonamide

HRID 2287360ノート

反応式

HRID 2287360 の反応式
[H-].[Na+].[C:3]1([CH:9]=[CH:10][S:11]([NH2:14])(=[O:13])=[O:12])[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[Cl:15][C:16]1[C:21]([O:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=2[O:29][CH3:30])=[C:20](Cl)[N:19]=[C:18]([C:32]2[N:37]=[CH:36][CH:35]=[CH:34][N:33]=2)[N:17]=1.Cl>CN(C)C=O>[Cl:15][C:16]1[N:17]=[C:18]([C:32]2[N:37]=[CH:36][CH:35]=[CH:34][N:33]=2)[N:19]=[C:20]([NH:14][S:11]([CH:10]=[CH:9][C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=2)(=[O:12])=[O:13])[C:21]=1[O:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=1[O:29][CH3:30]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 24758Sodium hydrideHCID 2575012-PhenylethenesulfonamideHCID 105457064,6-Dichloro-5-(2-methoxyphenoxy)-2,2'-bipyrimidine

生成物 1

HCID 53744388N-[6-chloro-5-(2-methoxyphenoxy)-2-(2-pyrimidinyl)-4-pyrimidinyl]-2-phenylethenesulfonamide収率 70.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Sodium hydride (60%) (480 mg) was added to a solution of 1.00 g of 2-phenylethenesulfonamide in 10 ml of dimethylformamide with ice cooling followed by stirring at room temperature for 15 minutes. To this reaction solution was added 1.91 g of 4,6-dichloro-5-(2-methoxyphenoxy)-2-(2-pyrimidinyl)-pyrimidine with stirring. The reaction mixture was stirred at room temperature for 2.5 hours and poured into a mixture of 1N hydrochloric acid and ice. The resulting crystals were collected by filtration and pulverized in hot ethanol. After allowing to cool, the crystals were collected by filtration to give 1.91 g of N-[6-chloro-5-(2-methoxyphenoxy)-2-(2-pyrimidinyl)-4-pyrimidinyl]-2-phenylethenesulfonamide.

後処理

  1. stirringwith stirring
  2. stirringThe reaction mixture was stirred at room temperature for 2.5 hours
  3. filtrationThe resulting crystals were collected by filtration
  4. temperatureto cool
  5. filtrationthe crystals were collected by filtration

出典と根拠

ORDレコード
ord-e1e7b0678d6c4405a758250dd1da664a
出典データセット
uspto-grants-2000_07
特許番号
US06083955

反応ノート

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