Potassium Carbonate → HCID 69217083, compound

HRID 272708Notes

Reaction equation

HRID 272708 reaction equation
[CH3:1][O:2][C:3]1[C:8]([O:9][CH2:10][O:11][CH2:12][CH2:13][Si:14]([CH3:17])([CH3:16])[CH3:15])=[CH:7][C:6]([NH:18]C(=O)C)=[C:5]([N+:22]([O-:24])=[O:23])[CH:4]=1.C([O-])([O-])=O.[K+].[K+]>CO>[CH3:1][O:2][C:3]1[C:8]([O:9][CH2:10][O:11][CH2:12][CH2:13][Si:14]([CH3:15])([CH3:17])[CH3:16])=[CH:7][C:6]([NH2:18])=[C:5]([N+:22]([O-:24])=[O:23])[CH:4]=1

Participants

4

Reactant 2

HCID 11430Potassium CarbonateHCID 69219020HCID 69219020, compound

Product 1

HCID 69217083HCID 69217083, compoundYield 91%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A mixture of Example 476D and K2CO3 (7.0 g, 50.6 mmol) in methanol (220 mL) was stirred at room temperature overnight, concentrated under vacuum, diluted with ethyl acetate, washed with water and brine, dried (MgSO4), filtered and concentrated under vacuum to produce 9.7 g (91%) of the desired product. MS (ESI) m/e 315 (M+H)+; 1H NMR (300 MHz, DMSO-d6) □ 7.43 (br s, 2H), 7.37 (s, 1H), 6.66 (s, 1H), 5.28 (s, 2H), 3.69-3.75 (m, 2H), 3.73 (s, 3H), 0.89-0.94 (m, 2H), -0.01 (s, 9H).

Workup

  1. concentrationconcentrated under vacuum
  2. additiondiluted with ethyl acetate
  3. washwashed with water and brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated under vacuum

Sources & evidence

ORD record
ord-abea9d7fdd3845df9b6ce056ca3c1c22
Source dataset
uspto-grants-2008_11
Patent number
US07456169B2

Reaction notes

Loading…