Hydrazine hydrate (1:1) → HCID 15003623, compound

HRID 1085646Notes

Reaction equation

HRID 1085646 reaction equation
Cl[C:2]1[C:7]([Cl:8])=[C:6]([O:9][CH3:10])[N:5]=[C:4]([CH3:11])[N:3]=1.O.[NH2:13][NH2:14]>O>[Cl:8][C:7]1[C:6]([O:9][CH3:10])=[N:5][C:4]([CH3:11])=[N:3][C:2]=1[NH:13][NH2:14]

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 15003621HCID 15003621, compound

Product 1

HCID 15003623HCID 15003623, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

4,5-Dichloro-6-methoxy-2-methylpyrimidine (21 g, 0.11 mol), 25 ml of hydrazine hydrate, and 25 ml of water were combined and heated to reflux for 25 min. The mixture was then cooled and extracted with methylene chloride. The extract was washed with water, dried over magnesium sulfate, and concentrated under reduced pressure. The solid residue was extracted with hexane and dried to obtain 12.8 g (62 percent of theory) of the title compound as a fluffy white solid melting at 158° C.-159° C.

Workup

  1. temperatureheated
  2. temperatureto reflux for 25 min
  3. temperatureThe mixture was then cooled
  4. extractionextracted with methylene chloride
  5. washThe extract was washed with water
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. extractionThe solid residue was extracted with hexane
  9. customdried

Sources & evidence

ORD record
ord-7ed81338fb494939a99cbd3f7fc6a092
Source dataset
uspto-grants-1991_04
Patent number
US05010195

Reaction notes

Loading…