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Ethanolamine → 2-[9-Ethyl-6-(3-fluoro-phenylamino)-9H-purin-2-ylamino]-ethanol

HRID 9912
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인쇄 미리보기

반응식

HRID 9912 반응식
Cl[C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH2:11][CH3:12])=[C:4]([NH:13][C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([F:20])[CH:15]=2)[N:3]=1.[CH2:21]([CH2:23][NH2:24])[OH:22]>C(OCC)(=O)C>[OH:22][CH2:21][CH2:23][NH:24][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH2:11][CH3:12])=[C:4]([NH:13][C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([F:20])[CH:15]=2)[N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 700EthanolamineHCID 219883192-chloro-9-ethyl-6-(3-fluoro-phenyl-amino)-9H-purine

생성물 1

HCID 219882472-[9-Ethyl-6-(3-fluoro-phenylamino)-9H-purin-2-ylamino]-ethanol

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

0.2 g (0.62 mmol) of 2-chloro-9-ethyl-6-(3-fluoro-phenyl-amino)-9H-purine (prepared according to Stage 90.2) is stirred in 1 ml of ethanolamine at 150° C. for 3 h, and the mixture is allowed to cool and is diluted with ethyl acetate. The organic phase is washed with water, separated off and dried over sodium sulfate. On concentration, 2-(2-hydroxy-ethyl-amino)-6-(3-fluoro-phenyl-amino)-9-ethyl-9H-purine is obtained as a crystalline precipitate. This precipitate is filtered off and dried; m.p. 184° C.; FAB-MS: (M+H)+=317; Rf=0.5 (CH2Cl2:methanol=9:1).

후처리

  1. temperatureto cool
  2. washThe organic phase is washed with water
  3. customseparated off
  4. dry with materialdried over sodium sulfate
  5. concentrationOn concentration

출처 및 근거

ORD 기록
ord-65634670e10c47c68865d9e95be13558
출처 데이터셋
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07091346B1

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