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

HRID 9897

반응식

HRID 9897 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
150 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-10cbb19efc2447da90278f6f11f5b438
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091346B1

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