Potassium Carbonate → HCID 21541521, compound

HRID 1076027Notes

Reaction equation

HRID 1076027 reaction equation
C([O:3][C:4](=[O:26])[CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]1[O:13][C:14]([CH2:17][CH2:18][CH:19]([OH:25])[CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])=[CH:15][CH:16]=1)C.C(=O)([O-])[O-].[K+].[K+]>CO>[OH:25][CH:19]([CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])[CH2:18][CH2:17][C:14]1[O:13][C:12]([CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][C:4]([OH:26])=[O:3])=[CH:16][CH:15]=1

Participants

4

Reactant 2

HCID 11430Potassium CarbonateHCID 54282569HCID 54282569, compound

Product 1

HCID 21541521HCID 21541521, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A mixture of VI (2.73 g, 0.00745 mole), methanol (100 ml), and 20% aqueous potassium carbonate solution (30 ml) was stirred and heated under reflux for 1 hour. The turbid solution was concentrated to 1/4 of the volume by distillation from a water bath (60°C) under reduced pressure (60 mm Hg). The residue was diluted with water (100 ml) and adjusted to pH 7 with acetic acid (2.7 ml). The resulting emulsion was extracted with two 80-ml portions of ether. The combined ethereal extracts were washed with water (100 ml) and then dried over magnesium sulfate. Ether was distilled off from a water bath (50°C), at last under 15 mm Hg. The yellow, oily residue (2.58 g) was purified by crystallization from petroleum ether (boiling below 50°C) (450 ml). 2.13 g (84%) of VIa were hereby obtained as almost white crystals with m.p. 43°-45°C.

Workup

  1. temperatureheated
  2. temperatureunder reflux for 1 hour
  3. concentrationThe turbid solution was concentrated to 1/4 of the volume by distillation from a water bath (60°C) under reduced pressure (60 mm Hg)
  4. additionThe residue was diluted with water (100 ml)
  5. extractionThe resulting emulsion was extracted with two 80-ml portions of ether
  6. washThe combined ethereal extracts were washed with water (100 ml)
  7. dry with materialdried over magnesium sulfate
  8. distillationEther was distilled off from a water bath (50°C)
  9. customThe yellow, oily residue (2.58 g) was purified by crystallization from petroleum ether (boiling below 50°C) (450 ml)
  10. custom2.13 g (84%) of VIa were hereby obtained as almost white crystals with m.p. 43°-45°C.

Sources & evidence

ORD record
ord-7bcd15b458074b41b2df317d9c7e07a9
Source dataset
uspto-grants-1976_05
Patent number
US03954813

Reaction notes

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