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

HRID 216240

反応式

HRID 216240 の反応式
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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
85 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b0de618506524590bcdeb5c36842485b
出典データセット
uspto-grants-2012_06
特許番号
US08193183B2

関連ノート

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