Piperazine → HCID 20150133, compound

HRID 568413Notes

Reaction equation

HRID 568413 reaction equation
[CH2:1]([S:3][C:4]1[C:9]2[N:10]=[C:11](Cl)[N:12]=[C:13]([N:14]3[CH2:19][CH2:18][S:17](=[O:20])[CH2:16][CH2:15]3)[C:8]=2[N:7]=[CH:6][N:5]=1)[CH3:2].[NH:22]1[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1>CS(C)=O.O>[CH2:1]([S:3][C:4]1[C:9]2[N:10]=[C:11]([N:22]3[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]3)[N:12]=[C:13]([N:14]3[CH2:19][CH2:18][S:17](=[O:20])[CH2:16][CH2:15]3)[C:8]=2[N:7]=[CH:6][N:5]=1)[CH3:2]

Participants

5

Reactant 2

HCID 4837PiperazineHCID 20150206HCID 20150206, compound

Product 1

HCID 20150133HCID 20150133, compound

Reagents, catalysts & solvents 2

HCID 679Dimethyl SulfoxideSolvent2×HCID 962WaterSolvent

Conditions

Temperature
40 °C

Procedure

A solution of 3, 4 gm (0.01 mol) of 8-ethylthio-2-chloro-4-(1-oxido-thiomorpholino)-pyrimido-[5,4-d]-pyrimidine (m.p. 197°-199° C.) in 100 ml of dimethylsulfoxide was slowly poured, while stirring, into a solution of 4.3 gm (0.05 mol) of piperazine in 75 ml of dimethylsulfoxide at 40° C., and the mixture was stirred for 1 hour at 40° C. The reaction mixture was then taken up in about 1 liter of water, whereby the reaction product slowly precipitated in crystalline form. After standing for a short period of time, the precipitate was suction-filtered off, washed with water and dried at about 70° C.

Workup

  1. customwhereby the reaction product slowly precipitated in crystalline form
  2. waitAfter standing for a short period of time
  3. filtrationthe precipitate was suction-filtered off
  4. washwashed with water
  5. customdried at about 70° C.

Sources & evidence

ORD record
ord-1cff866610cd4bd1a8b52b897747210a
Source dataset
uspto-grants-1988_03
Patent number
US04728646

Reaction notes

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