Trifluoroacetic acid → N2-(2-Cyclopropylethyl)-8-(methoxy)-9H-Purine-2,6-diamine trifluoroacetate

HRID 1011046Notes

Reaction equation

HRID 1011046 reaction equation
[CH:1]1([CH2:4][CH2:5][NH:6][C:7]2[N:15]=[C:14]3[C:10]([N:11]=[C:12]([O:22][CH3:23])[N:13]3C3CCCCO3)=[C:9]([NH2:24])[N:8]=2)[CH2:3][CH2:2]1.[F:25][C:26]([F:31])([F:30])[C:27]([OH:29])=[O:28]>CO>[F:25][C:26]([F:31])([F:30])[C:27]([OH:29])=[O:28].[CH:1]1([CH2:4][CH2:5][NH:6][C:7]2[N:15]=[C:14]3[C:10]([N:11]=[C:12]([O:22][CH3:23])[NH:13]3)=[C:9]([NH2:24])[N:8]=2)[CH2:3][CH2:2]1

Participants

4

Reactant 2

HCID 6422Trifluoroacetic acidHCID 57699615N2-(2-cyclopropylethyl)-8-(methoxy)-9-(tetrahydro-2H-pyran-2-yl)-9H-purine-2,6-diamine

Product 1

HCID 178493988N2-(2-Cyclopropylethyl)-8-(methoxy)-9H-Purine-2,6-diamine trifluoroacetate

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a solution of N2-(2-cyclopropylethyl)-8-(methoxy)-9-(tetrahydro-2H-pyran-2-yl)-9H-purine-2,6-diamine (3.30 g) in methanol (33.0 ml) at room temperature was added trifluoroacetic acid (3.30 ml) to give an orange solution. The reaction mixture was stirred at room temperature for 70 hours. The reaction mixture was concentrated in vacuo to give a yellow solid which was then triturated in diethyl ether (100 ml) and filtered under vacuum to give an off-white solid (2.4 g).

Workup

  1. customto give an orange solution
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. customto give a yellow solid which
  4. customwas then triturated in diethyl ether (100 ml)
  5. filtrationfiltered under vacuum

Sources & evidence

ORD record
ord-166ec5b7adb64e7e8007d6aa8c23f08e
Source dataset
uspto-grants-2011_07
Patent number
US07977344B2

Reaction notes

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