Water → HCID 68647784, compound

HRID 1163002Notes

Reaction equation

HRID 1163002 reaction equation
[CH3:1][C:2]([CH3:19])([CH3:18])[CH2:3][NH:4][C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[C:12]([OH:15])[CH:13]=2)[N:8]=[C:7]([C:16]#[N:17])[N:6]=1.Cl[CH2:21][CH2:22][CH2:23][N:24]1[CH2:29][CH2:28][N:27]([CH2:30][CH2:31]C)[CH2:26][CH2:25]1.[C:33](=O)([O-])[O-:34].[Cs+].[Cs+].O>CN(C=O)C>[CH3:1][C:2]([CH3:19])([CH3:18])[CH2:3][NH:4][C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[C:12]([O:15][CH2:21][CH2:22][CH2:23][N:24]3[CH2:29][CH2:28][N:27]([CH2:30][CH2:31][O:34][CH3:33])[CH2:26][CH2:25]3)[CH:13]=2)[N:8]=[C:7]([C:16]#[N:17])[N:6]=1

Participants

6

Reactant 4

HCID 962Water2×HCID 10796Cesium carbonateHCID 61287108HCID 61287108, compoundHCID 686472384-(2,2-Dimethyl-propylamino)-6-hydroxy-quinazoline-2-carbonitrile

Product 1

HCID 68647784HCID 68647784, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

4-(2,2-Dimethyl-propylamino)-6-hydroxy-quinazoline-2-carbonitrile (0.3 mmol), 1-(3-chloro-propyl)-4-propyl-piperazine (0.62 mmol) and cesium carbonate (3.1 mmol) are stirred in DMF (3 ml) at RT for 20 hours. Water is added until a clear solution is formed. Then more water is added until the solution gets turbide. The precipitate formed is filtered off, washed with water and dried (vacuum). A powder with mp. 92-94° C., Rf=0.45 (CH2Cl2/MeOH=9:2) is obtained.

Workup

  1. customis formed
  2. customThe precipitate formed
  3. filtrationis filtered off
  4. washwashed with water
  5. customdried (vacuum)
  6. customA powder with mp. 92-94° C., Rf=0.45 (CH2Cl2/MeOH=9:2) is obtained

Sources & evidence

ORD record
ord-936bc3e49e5341b6bf1d80a2dffccc14
Source dataset
uspto-grants-2010_10
Patent number
US07820818B2

Reaction notes

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