Sodium hydride → HCID 135778496, compound
Reaction equation
[H-].[Na+].[NH2:3][C:4]1[N:5]([CH2:25][CH2:26]Cl)[N:6]=[C:7]2[C:12]=1[C:11](=[O:13])[N:10]([CH2:14][CH2:15][CH3:16])[C:9](=[O:17])[N:8]2[CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>>[CH2:18]([N:8]1[C:7]2=[N:6][N:5]3[CH2:25][CH2:26][NH:3][C:4]3=[C:12]2[C:11](=[O:13])[N:10]([CH2:14][CH2:15][CH3:16])[C:9]1=[O:17])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1Participants
3
Procedure
Sodium hydride (60% oil, 0.8 g) was added in portions to a stirring solution of 3-amino-7-benzyl-2-(2-chloroethyl) -5-propyl-2H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione (4.9 g) under cooling with ice bath. The mixture was stirred for 17 hours and was concentrated to dryness. The residue was triturated with water and the resulting crystals were collected by filtration, washed with water and dried.
Workup
- temperatureunder cooling with ice bath
- concentrationwas concentrated to dryness
- customThe residue was triturated with water
- filtrationthe resulting crystals were collected by filtration
- washwashed with water
- customdried
Sources & evidence
- ORD record
- ord-c71be86405b247b8bea07e491fdc362e
- Source dataset
- uspto-grants-1991_07
- Patent number
- US05032594
Reaction notes
Loading…