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Potassium Carbonate → HCID 21258170, compound

HRID 635206
Notes
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Reaction equation

HRID 635206 reaction equation
[CH2:1]([N:8]1[C:16]2[C:15](=[O:17])[N:14]([CH2:18][CH2:19][CH3:20])[C:13](=[O:21])[NH:12][C:11]=2[N:10]=[C:9]1[C:22]([CH3:25])([CH3:24])[CH3:23])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([O-])([O-])=O.[K+].[K+].CS([CH2:36][CH2:37][C:38]([O:40][CH3:41])=[O:39])(=O)=O>CN(C)C=O>[CH2:1]([N:8]1[C:16]2[C:15](=[O:17])[N:14]([CH2:18][CH2:19][CH3:20])[C:13](=[O:21])[N:12]([CH2:36][CH2:37][C:38]([O:40][CH3:41])=[O:39])[C:11]=2[N:10]=[C:9]1[C:22]([CH3:24])([CH3:23])[CH3:25])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 5744053Methyl 3-(methylsulfonyl)propanoateHCID 21258176HCID 21258176, compound

Product 1

HCID 21258170HCID 21258170, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Conditions

Temperature
95 °C

Procedure

5.0 g (14.7 mmol) of 7-benzyl-8-(tert.-butyl)-1-n-propyl-xanthine are dissolved in 200 ml of dimethylformamide. After the addition of 5.36 g of K2CO3, 19.6 mmol of methyl 3-methanesulphonylpropionate are added at ambient temperature and the mixture is then heated to 90-100° C. After about 20 hours at constant temperature the solvent is distilled off in vacuo and the residue remaining is taken up in dichloromethane. The organic phase is washed with water, dried over MgSO4 and the solvent is distilled off in vacuo. The crude product remaining is purified by chromatography on silica gel (dichloromethane:methanol 97:3).

Workup

  1. additionare added at ambient temperature
  2. distillationAfter about 20 hours at constant temperature the solvent is distilled off in vacuo
  3. washThe organic phase is washed with water
  4. dry with materialdried over MgSO4
  5. distillationthe solvent is distilled off in vacuo
  6. customThe crude product remaining is purified by chromatography on silica gel (dichloromethane:methanol 97:3)

Sources & evidence

ORD record
ord-f13d4f34e21c4543b9b1d3bf8ce5a5f8
Source dataset
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06187780B1

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes