Acetic Anhydride → HCID 10149094, compound

HRID 969708Notes

Reaction equation

HRID 969708 reaction equation
[NH2:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][CH:7]=[N:8]2)=[C:4]([Cl:11])[N:3]=1.[C:12](OC(=O)C)(=[O:14])[CH3:13]>CN(C)C(=O)C>[C:12]([N:8]1[CH:7]=[N:6][C:5]2[C:9]1=[N:10][C:2]([NH2:1])=[N:3][C:4]=2[Cl:11])(=[O:14])[CH3:13]

Participants

4

Reactant 2

HCID 7918Acetic AnhydrideHCID 53603492-Amino-6-chloropurine

Product 1

HCID 10149094HCID 10149094, compoundYield 99.3%

Reagents, catalysts & solvents 1

HCID 31374DimethylacetamideSolvent

Conditions

Temperature
55 °C

Procedure

2-Amino-6-chloropurine (150 g, 0.89 mol) and acetic anhydride (108 g, 1.06 mol) were added to N,N-dimethylacetamide (350 ml), and the mixture was heated to 50-60° C. and stirred for 4 hr. The reaction mixture was cooled and filtrated. The obtained crystals were washed with isopropanol (400 ml) and dried at 80° C. under reduced pressure to give 9-acetyl-2-amino-6-chloropurine as a pale-yellow powder (187 g, yield 99.0%).

Workup

  1. temperatureThe reaction mixture was cooled
  2. filtrationfiltrated
  3. washThe obtained crystals were washed with isopropanol (400 ml)
  4. customdried at 80° C. under reduced pressure

Sources & evidence

ORD record
ord-b970f82ee60a4c619af40a56fe96965c
Source dataset
uspto-grants-2007_12
Patent number
US07307167B2

Reaction notes

Loading…