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

HRID 2287360노트

반응식

HRID 2287360 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e1e7b0678d6c4405a758250dd1da664a
출처 데이터셋
uspto-grants-2000_07
특허 번호
US06083955

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