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Cesium carbonate → 4-Cyclopentylamino-6-[2-(4-methyl-piperazin-1-yl)-ethoxy]-quinazoline-2-carbonitrile

HRID 1163000
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HRID 1163000 반응식
[CH:1]1([NH:6][C:7]2[C:16]3[C:11](=[CH:12][CH:13]=[C:14]([OH:17])[CH:15]=3)[N:10]=[C:9]([C:18]#[N:19])[N:8]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1.Cl.Cl.Cl[CH2:23][CH2:24][N:25]1[CH2:30][CH2:29][N:28]([CH3:31])[CH2:27][CH2:26]1.C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C=O)C>[CH:1]1([NH:6][C:7]2[C:16]3[C:11](=[CH:12][CH:13]=[C:14]([O:17][CH2:23][CH2:24][N:25]4[CH2:30][CH2:29][N:28]([CH3:31])[CH2:27][CH2:26]4)[CH:15]=3)[N:10]=[C:9]([C:18]#[N:19])[N:8]=2)[CH2:2][CH2:3][CH2:4][CH2:5]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 111839401-(2-Chloroethyl)-4-methylpiperazine dihydrochlorideHCID 686476604-Cyclopentylamino-6-hydroxy-quinazoline-2-carbonitrile

생성물 1

HCID 686473854-Cyclopentylamino-6-[2-(4-methyl-piperazin-1-yl)-ethoxy]-quinazoline-2-carbonitrile

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

4-Cyclopentylamino-6-hydroxy-quinazoline-2-carbonitrile (0.4 mmol), 1-(2-Chloro-ethyl)-4-methyl-piperazine dihydrochloride (0.55 mmol) and cesium carbonate (4 mmol) are stirred in DMF (5 ml) at RT for 20 hours. The suspension is filtered, washed with little DMF and water is added to the filtrate until the solution gets turbide. The precipitate formed is filtered off, washed with water and dried (vacuum). A powder with mp. 110-112° C., Rf=0.48 (CH2Cl2/MeOH=9:2) is obtained.

후처리

  1. filtrationThe suspension is filtered
  2. washwashed with little DMF and water
  3. additionis added to the filtrate until the solution
  4. customThe precipitate formed
  5. filtrationis filtered off
  6. washwashed with water
  7. customdried (vacuum)
  8. customA powder with mp. 110-112° C., Rf=0.48 (CH2Cl2/MeOH=9:2) is obtained

출처 및 근거

ORD 기록
ord-3a620245a6944a0fba9747ea93943d11
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07820818B2

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