Dichloromethane → HCID 178496341, compound

HRID 26445Notes

Reaction equation

HRID 26445 reaction equation
[NH2:1][C:2]1[N+:7]([O-:8])=[C:6]([NH2:9])[CH:5]=[C:4]([N:10]2[CH2:15][CH:14]=[CH:13][CH2:12][CH2:11]2)[N:3]=1.C(Cl)Cl.[CH3:19][O:20][CH2:21][CH2:22][O:23][C:24](Cl)=[O:25]>C(N(CC)CC)C>[N:10]1([C:4]2[N:3]=[C:2]([NH:1][C:24]([O:23][CH2:22][CH2:21][O:20][CH3:19])=[O:25])[N+:7]([O-:8])=[C:6]([NH:9][C:24]([O:23][CH2:22][CH2:21][O:20][CH3:19])=[O:25])[CH:5]=2)[CH2:11][CH:12]=[CH:13][CH2:14][CH2:15]1

Participants

5

Reactant 3

HCID 6344DichloromethaneHCID 694002-Methoxyethyl chloroformateHCID 178507852HCID 178507852, compound

Product 1

HCID 178496341HCID 178496341, compound

Reagents, catalysts & solvents 1

HCID 8471TriethylamineSolvent

Procedure

10 G. of 2,4-diamino-6-[3,6-dihydro-1(2H)-pyridyl]-pyrimidine-3-oxide are stirred at 5° C. in 150 ml. of methylene chloride and 30 ml. of triethylamine and treated with 20 ml. of chloroformic acid 2-methoxyethyl ester. The mixture is stirred at room temperature for 4 hours, then washed with water and extracted with methylene chloride. The organic phases are evaporated under reduced pressure and the residue is recrystallized from diethyl ether, there being obtained bis(2-methoxyethyl) 6-[3,6-dihydro-1(2H)-pyridyl]-2,4-pyrimidine-dicarbamate-3-oxide, having a melting point of 126°-128° C.

Workup

  1. washwashed with water
  2. extractionextracted with methylene chloride
  3. customThe organic phases are evaporated under reduced pressure
  4. customthe residue is recrystallized from diethyl ether, there

Sources & evidence

ORD record
ord-e692b1acb2a5489b9ba6844e903683e5
Source dataset
uspto-grants-1979_04
Patent number
US04150132

Reaction notes

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