Water → HCID 23154978, compound

HRID 1912847Notes

Reaction equation

[NH2:1][C:2]1[N:10]=[CH:9][N:8]=[C:7]2[C:3]=1[N:4]=[CH:5][N:6]2[C:11]1[CH:16]=[CH:15][C:14]([NH:17][C:18]([NH:20][C:21]2[CH:26]=[CH:25][C:24]([Cl:27])=[C:23]([C:28]([F:31])([F:30])[F:29])[CH:22]=2)=[O:19])=[CH:13][CH:12]=1.C([O-])(=O)C.[Na+].[Br:37]Br.O>C(O)(=O)C>[NH2:1][C:2]1[N:10]=[CH:9][N:8]=[C:7]2[C:3]=1[N:4]=[CH:5][N:6]2[C:11]1[CH:12]=[CH:13][C:14]([NH:17][C:18]([NH:20][C:21]2[CH:26]=[CH:25][C:24]([Cl:27])=[C:23]([C:28]([F:30])([F:31])[F:29])[CH:22]=2)=[O:19])=[C:15]([Br:37])[CH:16]=1

Participants

Conditions

Temperature: 50 °C

Procedure

In 30 mL of acetic acid, 1 g (2.23 mmol) of 1-[4-(6-aminopurin-9-yl)phenyl]-3-(4-chloro-3-(trifluoromethyl)phenyl)urea and 0.8 g (9.75 mmol) of sodium acetate were dissolved and to the solution, 0.7 g (4.38 mmol) of bromine was added dropwise and the mixture solution was stirred at 50° C. for one hour. To the reaction solution, 40 mL of water was added, and the deposited product was collected by filtration, and recrystallized from ethanol to obtain 1.095 g (93%) of a target product as a white solid.

Workup

additionwas added dropwise
filtrationthe deposited product was collected by filtration
customrecrystallized from ethanol

Sources & evidence

ORD record: ord-b2a27d07f5d54881a251168b95e73805
Source dataset: uspto-grants-2013_12
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08609656B2

Reaction notes

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