1-Methylpiperazine → (2-Chloro-9-cyclopentyl-purin-6-yl)-{2-[3-(4-methyl-piperazin-1-yl)-propoxy]-phenyl}-amine

HRID 1984218노트

반응식

HRID 1984218 반응식
Cl[CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[NH:12][C:13]1[N:21]=[C:20]([Cl:22])[N:19]=[C:18]2[C:14]=1[N:15]=[CH:16][N:17]2[CH:23]1[CH2:27][CH2:26][CH2:25][CH2:24]1.[CH3:28][N:29]1[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]1>O>[Cl:22][C:20]1[N:19]=[C:18]2[C:14]([N:15]=[CH:16][N:17]2[CH:23]2[CH2:27][CH2:26][CH2:25][CH2:24]2)=[C:13]([NH:12][C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[O:5][CH2:4][CH2:3][CH2:2][N:32]2[CH2:33][CH2:34][N:29]([CH3:28])[CH2:30][CH2:31]2)[N:21]=1

참가 물질

4

반응물 2

HCID 531671-MethylpiperazineHCID 11774121HCID 11774121, 화합물

생성물 1

HCID 11784673(2-Chloro-9-cyclopentyl-purin-6-yl)-{2-[3-(4-methyl-piperazin-1-yl)-propoxy]-phenyl}-amine

시약·촉매·용매 1

HCID 962Water용매

실험 절차

[2-(3-Chloro-propoxy)-phenyl]-(2-chloro-9-cyclopentyl-purin-6-yl)-amine (0.4 mmol) are stirred at RT in N-methylpiperazine (0.3 ml) for 12 hours. The mixture is diluted with water and extracted 3 times with ethyl acetate. The combined organic phases are washed with brine and the extract is dried over sodium sulfate and evaporated. The residue is purified by flash chromatography on silica gel with (CH2Cl2/MeOH=9:1) as mobile phase. The product containing fractions are combined and evaporated. A pale oil with Rf=0.25 (CH2Cl2/MeOH=9:2) is obtained.

후처리

  1. extractionextracted 3 times with ethyl acetate
  2. washThe combined organic phases are washed with brine
  3. dry with materialthe extract is dried over sodium sulfate
  4. customevaporated
  5. customThe residue is purified by flash chromatography on silica gel with (CH2Cl2/MeOH=9:1) as mobile phase
  6. additionThe product containing fractions
  7. customevaporated
  8. customA pale oil with Rf=0.25 (CH2Cl2/MeOH=9:2) is obtained

출처 및 근거

ORD 기록
ord-38b3b222295e4edebf11192fcf6fabe1
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07544688B2

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