Potassium Hydroxide → HCID 13773257, compound

HRID 1651445Notes

Reaction equation

HRID 1651445 reaction equation
C([S:4][CH2:5][CH2:6][C:7]([N:9]1[N:13]=[C:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[S:11][CH:10]1[C:20]([O:22]CC)=[O:21])=[O:8])(=O)C.[OH-].[K+]>CO.O>[SH:4][CH2:5][CH2:6][C:7]([N:9]1[N:13]=[C:12]([C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)[S:11][CH:10]1[C:20]([OH:22])=[O:21])=[O:8]

Participants

5

Reactant 2

HCID 14797Potassium HydroxideHCID 13773256HCID 13773256, compound

Product 1

HCID 13773257HCID 13773257, compoundYield 33.3%

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 962WaterSolvent

Procedure

A solution of the product of step (b) (2.6g) in methanol (20ml) was cooled to 0° under nitrogen and treated dropwise with a solution of potassium hydroxide (1.42g) in water (8ml). The mixture was allowed to warm to room temperature over 2 hours and then partitioned between ethyl acetate and water. The aqueous phase was acidified with 2N HCl and the organic phase separated, washed with water and dried. Evaporation yielded an oil which slowly crystallised to give the title product (0.7g) as white crystals. mp 145°-6°.

Workup

  1. custompartitioned between ethyl acetate and water
  2. customthe organic phase separated
  3. washwashed with water
  4. customdried
  5. customEvaporation
  6. customyielded an oil which
  7. customslowly crystallised

Sources & evidence

ORD record
ord-48b3faa5e183425684f906c512ce5596
Source dataset
uspto-grants-1990_05
Patent number
US04927822

Reaction notes

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