Formic Acid → HCID 178525759, compound
Reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[CH2:17][C:16]2[C:11](=[N:12][C:13]([NH:18][C@H:19]3[CH2:24][CH2:23][C@H:22]([OH:25])[CH2:21][CH2:20]3)=[N:14][CH:15]=2)[NH:10][C:9]1=[O:26].[CH:27](O)=[O:28]>>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[CH2:17][C:16]2[C:11](=[N:12][C:13]([NH:18][C@H:19]3[CH2:20][CH2:21][C@H:22]([O:25][CH:27]=[O:28])[CH2:23][CH2:24]3)=[N:14][CH:15]=2)[NH:10][C:9]1=[O:26]Participants
3
Conditions
- Temperature
- 60 °C
Procedure
A mixture of 3-(2-chlorophenyl)-7-(trans-4-hydroxycyclohexylamino)-3,4-dihydropyrimido[4,5-d]pyrimidin-2(1H)-one (300 mg, 0.8 mal) (prepared as described in Example 73) and 96% formic acid (2 mL) was stirred at 60° C. for 3 hours, then concentrated under reduced pressure. The residue was triturated in ether, filtered and dried to give 250 mg of 3-(2-chlorophenyl)-7-(trans-4-formyloxycyclohexylamino)-3,4-dihydropyrimido[4,5-d]pyrimidin-2(1H)-one.
Workup
- concentrationconcentrated under reduced pressure
- customThe residue was triturated in ether
- filtrationfiltered
- customdried
Sources & evidence
- ORD record
- ord-a41da4258db744eb8fe3b60d2c927b8e
- Source dataset
- uspto-grants-2002_09
- Patent number
- US06451804B1
Reaction notes
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