HCID 135501905, compound → HCID 135493097, compound

HRID 2261070Notes

Reaction equation

HRID 2261070 reaction equation
FC(F)(F)C(O)=O.[NH2:8][C:9]1[NH:10][C:11](=[O:29])[C:12]2[N:13]=[CH:14][N:15]([CH2:18][O:19][CH2:20][CH2:21][O:22][C:23]([C:25]3([NH2:28])[CH2:27][CH2:26]3)=[O:24])[C:16]=2[N:17]=1>CO>[NH2:8][C:9]1[NH:10][C:11](=[O:29])[C:12]2[N:13]=[CH:14][N:15]([CH2:18][O:19][CH2:20][CH2:21][O:22][C:23]([C:25]3([NH2:28])[CH2:27][CH2:26]3)=[O:24])[C:16]=2[N:17]=1

Participants

3

Reactant 1

HCID 135501905HCID 135501905, compound

Product 1

HCID 135493097HCID 135493097, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

Dissolve 1-amino-cyclopropanecarboxylic acid 2-(2-amino-6-oxo-1,6-dihydro-purin-9-ylmethoxy)-ethyl ester trifluoroacetic acid salt (0.02 g, 0.05 mmol) of Example 1 in 1 mL methanol. Apply this solution to a 1 g Varian Mega Bond Elute® SCX column (Varian Part# 170532) pre-washed several times with methanol. Wash the column with 10 mL of methanol then elute the compound with 15 mL of a 2 M solution of ammonia in methanol. Concentrate in vacuo to obtain the desired free base as a white solid. MS (ES+): 309.2 (M+1)

Workup

  1. washApply this solution to a 1 g Varian Mega Bond Elute® SCX column (Varian Part# 170532)
  2. washpre-washed several times with methanol
  3. washWash the column with 10 mL of methanol
  4. washthen elute the compound with 15 mL of a 2 M solution of ammonia in methanol
  5. concentrationConcentrate in vacuo

Sources & evidence

ORD record
ord-c5dd167fc3314c4691a5296234b948c6
Source dataset
uspto-grants-2010_12
Patent number
US07846937B2

Reaction notes

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