Water → HCID 66754643, compound

HRID 1924403Notes

Reaction equation

HRID 1924403 reaction equation
[C:1]([CH2:3][O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[C:11](=O)[CH2:12][N:13]1[C:22](=[O:23])[C:21]2[N:20]([CH2:24][C:25]#[C:26][CH3:27])[C:19]([N:28]3[CH2:33][CH2:32][CH2:31][CH:30]([NH:34][C:35]([O:37][C:38]([CH3:41])([CH3:40])[CH3:39])=[O:36])[CH2:29]3)=[N:18][C:17]=2[N:16]([CH3:42])[C:14]1=[O:15])#[N:2].C(=O)([O-])[O-].[Cs+].[Cs+].O>CN(C)C=O>[C:1]([C:3]1[O:4][C:5]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=2[C:11]=1[CH2:12][N:13]1[C:22](=[O:23])[C:21]2[N:20]([CH2:24][C:25]#[C:26][CH3:27])[C:19]([N:28]3[CH2:33][CH2:32][CH2:31][CH:30]([NH:34][C:35]([O:37][C:38]([CH3:41])([CH3:40])[CH3:39])=[O:36])[CH2:29]3)=[N:18][C:17]=2[N:16]([CH3:42])[C:14]1=[O:15])#[N:2]

Participants

5

Reactant 3

HCID 962WaterHCID 10796Cesium carbonateHCID 66753435HCID 66753435, compound

Product 1

HCID 66754643HCID 66754643, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Conditions

Temperature
50 °C

Procedure

A mixture of 215 mg of 1-{2-[2-cyanomethoxy-phenyl]-2-oxo-ethyl}-3-methyl-7-(2-butyn-1-yl)-8-[3-(tert.-butyloxycarbonylamino)-piperidin-1-yl]-xanthine and 244 mg of caesium carbonate in 4 ml of N,N-dimethylformamide is stirred for two hours at 50° C., then a further three hours at 70° C. For working up the reaction mixture is combined with water and the precipitate formed is suction filtered and dried.

Workup

  1. customa further three hours
  2. customat 70° C
  3. customthe precipitate formed
  4. filtrationfiltered
  5. customdried

Sources & evidence

ORD record
ord-4a5a62aaa6da4a45933533867595b44e
Source dataset
uspto-grants-2012_05
Patent number
US08178541B2

Reaction notes

Loading…