Water → HCID 13592645, compound

HRID 986621Notes

Reaction equation

HRID 986621 reaction equation
Cl[C:2]1[N:3]=[C:4]([N:14]2[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)[C:5]2[N:11]=[CH:10][N:9]=[C:8]([S:12][CH3:13])[C:6]=2[N:7]=1.[NH:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1.O>CS(C)=O>[CH3:13][S:12][C:8]1[C:6]2[N:7]=[C:2]([N:20]3[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]3)[N:3]=[C:4]([N:14]3[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]3)[C:5]=2[N:11]=[CH:10][N:9]=1

Participants

5

Reactant 3

HCID 962WaterHCID 4837PiperazineHCID 13592631HCID 13592631, compound

Product 1

HCID 13592645HCID 13592645, compound

Reagents, catalysts & solvents 1

HCID 679Dimethyl SulfoxideSolvent2×

Procedure

2.0 g (6.8 mmol) of 2-chloro-8-methylthio-4-piperidino-pyrimido[5,4-d]pyrimidine is dissolved warm in 70 ml of dimethylsulphoxide and stirred with a solution of 6 g of piperazine in 70 ml of dimethylsulphoxide for 1 hour at ambient temperature. Then the solution is poured into 1 liter of water, the precipitate obtained is suction filtered and washed with water. The residue is taken up in 50 ml of methylene chloride and extracted with 50 ml of 0.05N sodium hydroxide solution. The organic phase is separated off, dried over sodium sulphate and concentrated in a rotary evaporator.

Workup

  1. customthe precipitate obtained
  2. filtrationfiltered
  3. washwashed with water
  4. extractionextracted with 50 ml of 0.05N sodium hydroxide solution
  5. customThe organic phase is separated off
  6. dry with materialdried over sodium sulphate
  7. concentrationconcentrated in a rotary evaporator

Sources & evidence

ORD record
ord-581cd6e0cc6044579623a7098e641123
Source dataset
uspto-grants-1987_12
Patent number
US04714698

Reaction notes

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