Water → (6-Chloro-2-methylsulfanyl-pyrimidin-4-yl)-[2-(2,4-dichloro-phenyl)-ethyl]-amine

HRID 216240

반응식

HRID 216240 반응식
Cl[C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[C:4]([S:9][CH3:10])[N:3]=1.[Cl:11][C:12]1[CH:17]=[C:16]([Cl:18])[CH:15]=[CH:14][C:13]=1[CH2:19][CH2:20][NH2:21].C(=O)(O)[O-].[Na+].O>CCO>[Cl:8][C:6]1[N:5]=[C:4]([S:9][CH3:10])[N:3]=[C:2]([NH:21][CH2:20][CH2:19][C:13]2[CH:14]=[CH:15][C:16]([Cl:18])=[CH:17][C:12]=2[Cl:11])[CH:7]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 805314,6-Dichloro-2-(methylthio)pyrimidineHCID 1429382,4-DichlorophenethylamineHCID 516892Sodium Bicarbonate

생성물 1

HCID 80545555(6-Chloro-2-methylsulfanyl-pyrimidin-4-yl)-[2-(2,4-dichloro-phenyl)-ethyl]-amine수율 72.3%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
85 °C

실험 절차

A mixture of 4,6-dichloro-2-methylsulfanyl-pyrimidine (2.66 g, 13.6 mmol), 2-(2,4-dichloro-phenyl)-ethylamine (2.26 mL, 15 mmol) and sodium bicarbonate (2.29 g, 27.2 mmol) in EtOH (35 mL) is heated to 85° C. for 1 hour and poured into water (100 mL). The solid precipitate is collected by filtration and dissolved in hot EtOH (75 mL). After cooling overnight the crystals that formed are collected by filtration and dried to afford (6-chloro-2-methylsulfanyl-pyrimidin-4-yl)-[2-(2,4-dichloro-phenyl)-ethyl]-amine (3.43 g, 72%) as a solid.

후처리

  1. filtrationThe solid precipitate is collected by filtration
  2. dissolutiondissolved in hot EtOH (75 mL)
  3. temperatureAfter cooling overnight the crystals
  4. customthat formed
  5. filtrationare collected by filtration
  6. customdried

출처 및 근거

ORD 기록
ord-b0de618506524590bcdeb5c36842485b
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08193183B2

연결된 노트

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