Methanesulfonic acid--6-chloro-7H-purine (1/1) → 6-Chloropurine

HRID 1995740Notes

Reaction equation

HRID 1995740 reaction equation
CS(O)(=O)=O.[Cl:6][C:7]1[N:15]=[CH:14][N:13]=[C:12]2[C:8]=1[NH:9][CH:10]=[N:11]2>O>[Cl:6][C:7]1[N:15]=[CH:14][N:13]=[C:12]2[C:8]=1[NH:9][CH:10]=[N:11]2

Participants

3

Reactant 1

HCID 20487940Methanesulfonic acid--6-chloro-7H-purine (1/1)

Product 1

HCID 53592776-ChloropurineYield 84.3%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

To 15 ml of water there were added 5 g of 6-chloropurine methansulfonate with vigorous stirring. After stirring for 15 minutes at room temperature the mixture was allowed to stand in a freezer for 1 hour after which the light yellow precipitate which formed was collected by filtration. The filter cake was washed with 5 ml of ice water and dried in a vacuum oven at 55° C. to give 2.6 g (84% yield) of 6-chloropurine, λ max (H2O)=265 nm, ε=9.22×103.

Workup

  1. waitto stand in a freezer for 1 hour
  2. customafter which the light yellow precipitate which formed
  3. filtrationwas collected by filtration
  4. washThe filter cake was washed with 5 ml of ice water
  5. customdried in a vacuum oven at 55° C.

Sources & evidence

ORD record
ord-b1d4d25ef7b24a15b12377ff3b20f158
Source dataset
uspto-grants-1983_09
Patent number
US04405781

Reaction notes

Loading…