Cesium carbonate → 4-Cyclopentylamino-6-(2-dimethylamino-ethoxy)-quinazoline-2-carbonitrile

HRID 1984224노트

반응식

HRID 1984224 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[CH2:22][CH2:23][N:24]([CH3:26])[CH3:25].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][CH2:22][CH2:23][N:24]([CH3:26])[CH3:25])[CH:15]=3)[N:10]=[C:9]([C:18]#[N:19])[N:8]=2)[CH2:2][CH2:3][CH2:4][CH2:5]1

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 11636816N,N-Dimethylaminoethyl chloride hydrochlorideHCID 686476604-Cyclopentylamino-6-hydroxy-quinazoline-2-carbonitrile

생성물 1

HCID 686473294-Cyclopentylamino-6-(2-dimethylamino-ethoxy)-quinazoline-2-carbonitrile

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

4-Cyclopentylamino-6-hydroxy-quinazoline-2-carbonitrile (0.4 mmol), (2-Chloro-ethyl)-dimethyl-amine hydrochloride (0.55 mmol) and cesiumcarbonate (3.5 mmol) are stirred in DMF (3 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 and dried (vacuum). A white powder with mp. 158-160° C., Rf=0.51 (CH2C2/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. customdried (vacuum)
  7. customA white powder with mp. 158-160° C., Rf=0.51 (CH2C2/MeOH=9:2) is obtained

출처 및 근거

ORD 기록
ord-bba5bae372c44bb0adf9eb6de3e91342
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07544688B2

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