Ammonia → HCID 13649692, compound

HRID 1248886Notes

Reaction equation

HRID 1248886 reaction equation
[Cl:1][C:2]1[CH:7]=[C:6](Cl)[N:5]=[C:4]([NH:9][CH2:10][CH2:11][CH2:12][O:13][CH3:14])[N:3]=1.[NH3:15]>O1CCOCC1>[NH2:15][C:6]1[CH:7]=[C:2]([Cl:1])[N:3]=[C:4]([NH:9][CH2:10][CH2:11][CH2:12][O:13][CH3:14])[N:5]=1

Participants

4

Reactant 2

HCID 222AmmoniaHCID 136496914,6-Dichloro-N-(3-methoxypropyl)pyrimidin-2-amine

Product 1

HCID 13649692HCID 13649692, compoundYield 61.6%

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

10 g (0.042 mole) of 4,6-dichloro-2-(3-methoxypropylamino)-pyrimidine are dissolved in 100 ml of dioxane and 60 ml of aqueous ammonia solution are added. After the reaction mixture has been heated to the boil for four hours, it is mixed with 1 liter of ice water and extracted with methylene chloride. The extract is dried over sodium sulphate and concentrated, and the residue which remains is boiled up with white spirit, filtered off and dried. 5.6 g (61.6% of theory) of the desired pyrimidine, melting point 141° C., are obtained.

Workup

  1. temperatureAfter the reaction mixture has been heated to the boil for four hours
  2. extractionextracted with methylene chloride
  3. dry with materialThe extract is dried over sodium sulphate
  4. concentrationconcentrated
  5. filtrationfiltered off
  6. customdried

Sources & evidence

ORD record
ord-333677121e9846a6812a0b3a2f868ed8
Source dataset
uspto-grants-1986_12
Patent number
US04627872

Reaction notes

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