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

HRID 1162999ノート

反応式

HRID 1162999 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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 (CH2Cl2/MeOH=9:2) is obtained.

後処理

  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 (CH2Cl2/MeOH=9:2) is obtained

出典と根拠

ORDレコード
ord-dbbcce92ff374b5896719d21ce4951d4
出典データセット
uspto-grants-2010_10
特許番号
US07820818B2

反応ノート

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