Ethylenediamine → 2-(2-Amino-ethylamino)-6-(3-chloro-phenyl-amino)-9-isopropyl-9H-purine

HRID 9897

反応式

HRID 9897 の反応式
Cl[C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH:11]([CH3:13])[CH3:12])=[C:4]([NH:14][C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([Cl:21])[CH:16]=2)[N:3]=1.[CH2:22]([NH2:25])[CH2:23][NH2:24]>C(OCC)(=O)C>[NH2:24][CH2:23][CH2:22][NH:25][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH:11]([CH3:13])[CH3:12])=[C:4]([NH:14][C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([Cl:21])[CH:16]=2)[N:3]=1

参加物

4

反応物 2

HCID 3301EthylenediamineHCID 219882482-Chloro-N-(3-chlorophenyl)-9-isopropyl-9H-purin-6-amine

生成物 1

HCID 219882262-(2-Amino-ethylamino)-6-(3-chloro-phenyl-amino)-9-isopropyl-9H-purine

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
150 °C

実験手順

200 mg (0.58 mmol) of 2-chloro-6-(3-chloro-phenyl-amino)-9-isopropyl-9H-purine are dissolved in 6 ml (90 mmol) of ethylenediamine and the mixture is heated under reflux for 3 hours (oil bath temperature of 150° C.). After cooling to room temperature, the reaction mixture is taken up in 250 ml of ethyl acetate and extracted with 150 ml of water. The aqueous phase is extracted twice with ethyl acetate and the combined organic extracts are washed with saturated sodium bicarbonate solution, water and saturated sodium chloride solution and dried over magnesium sulfate. After filtration, the filtrate is concentrated under reduced pressure at 35° C. and dried under an HV. 2-(2-Amino-ethylamino)-6-(3-chloro-phenyl-amino)-9-isopropyl-9H-purine is obtained; Rf=0.27 (methylene chloride:methanol:concentrated ammonium hydroxide solution=900:100:1); EI-MS: (M+H)+=346; m.p. 55–56° C.

後処理

  1. temperaturethe mixture is heated
  2. temperatureAfter cooling to room temperature
  3. extractionextracted with 150 ml of water
  4. extractionThe aqueous phase is extracted twice with ethyl acetate
  5. washthe combined organic extracts are washed with saturated sodium bicarbonate solution, water and saturated sodium chloride solution
  6. dry with materialdried over magnesium sulfate
  7. filtrationAfter filtration
  8. concentrationthe filtrate is concentrated under reduced pressure at 35° C.
  9. customdried under an HV

出典と根拠

ORDレコード
ord-10cbb19efc2447da90278f6f11f5b438
出典データセット
uspto-grants-2006_08
特許番号
US07091346B1

関連ノート

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