Ethanol → HCID 178507684, compound

HRID 2052072Notes

Reaction equation

HRID 2052072 reaction equation
[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[C:4]([Cl:9])[N:3]=1.C([OH:12])C.ClC1C=CC=C(C(OO)=O)C=1.[OH-].[Na+]>O>[NH2:1][C:2]1[N+:7]([O-:12])=[C:6]([NH2:8])[CH:5]=[C:4]([Cl:9])[N:3]=1

Participants

6

Reactant 4

HCID 702Ethanol2×HCID 14798Sodium HydroxideHCID 674322,4-Diamino-6-chloropyrimidineHCID 70297m-Chloroperbenzoic acid

Product 1

HCID 178507684HCID 178507684, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
-10 °C

Procedure

75 G. of 2,4-diamino-6-chloropyrimidine are dissolved in 1500 ml. of ethanol at 35° C. The solution is cooled to -10° C. and a solution of 100 g. of 3-chloroperbenzoic acid in 500 ml. of ethanol is slowly added dropwise in the course of 1 hour. The suspension is subsquently stirred at -10° C. for 7 hours and left stand at 5° C. overnight. The suspension is neutralized with 24 g. of sodium hydroxide in100 ml. of water. The solid material is filtered off and recrystallized from ethanol, there being obtained pure 2,4-diamino-6-chloropyrimidine-3-oxide.

Workup

  1. customat 35° C
  2. waitleft stand at 5° C. overnight
  3. filtrationThe solid material is filtered off
  4. customrecrystallized from ethanol, there

Sources & evidence

ORD record
ord-5de027be26024b978a313b965d3e6260
Source dataset
uspto-grants-1980_01
Patent number
US04182867

Reaction notes

Loading…