Acetic Acid → HCID 10542766, compound

HRID 1957192Notes

Reaction equation

HRID 1957192 reaction equation
[OH-].[K+].[CH2:3]([N:10]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[C:12]2[CH:19]=[C:20]([C:22]([O:24]C)=[O:23])[S:21][C:11]1=2)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.C(O)(=O)C>CO.O>[CH2:3]([N:10]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[C:12]2[CH:19]=[C:20]([C:22]([OH:24])=[O:23])[S:21][C:11]1=2)[C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1

Participants

5

Reactant 3

HCID 176Acetic AcidHCID 14797Potassium HydroxideHCID 10615766HCID 10615766, compound

Product 1

HCID 10542766HCID 10542766, compound

Reagents, catalysts & solvents 1

HCID 22242641Methanol--water (1/1)Solvent

Procedure

KOH (3 g) was dissolved in methanol-water (1/1) (50 ml). (5) (3 g) was added and the mixture refluxed until the compound was in solution and subsequently 1 h in addition. After cooling the mixture was acidified with acetic acid to pH=6, and the mixture was stirred overnight. The formed precipitate was filtered off, washed with water and dried in vacuo at 50° C. The crude product (3 g) was boiled in water once more, cooled, filtered and dried again giving analytically pure (8), m.p. 194°-195° C.

Workup

  1. temperaturethe mixture refluxed until the compound
  2. customwas in solution and subsequently 1 h in addition
  3. temperatureAfter cooling the mixture
  4. filtrationThe formed precipitate was filtered off
  5. washwashed with water
  6. customdried in vacuo at 50° C
  7. temperaturecooled
  8. filtrationfiltered
  9. customdried again

Sources & evidence

ORD record
ord-1d32920ebf8b43839bf9d38610773ed7
Source dataset
uspto-grants-1998_07
Patent number
US05783575

Reaction notes

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