HCID 54127341, compound → HCID 19350794, compound

HRID 1636298Notes

Reaction equation

HRID 1636298 reaction equation
[CH2:1]([O:8][CH2:9][CH:10]([CH2:16][OH:17])[O:11][CH2:12][C:13]([OH:15])=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>C1C=CC=CC=1.S(=O)(=O)(O)O>[CH2:1]([O:8][CH2:9][CH:10]1[CH2:16][O:17][C:13](=[O:15])[CH2:12][O:11]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Participants

4

Reactant 1

HCID 54127341HCID 54127341, compound

Product 1

HCID 19350794HCID 19350794, compound

Reagents, catalysts & solvents 2

HCID 1118Sulfuric AcidCatalystHCID 241BenzeneSolvent

Procedure

Hydroxy acid (2.34 g) obtained from Example 27 was dissolved in benzene (400 ml), and concentrated sulfuric acid (4 drops) was added thereto. The reaction mixture was stirred under reflux for 2 hours as removing water by Dean-Stark trap to complete the reaction. The reaction mixture was washed with water and saturated brine sequentially and dried over anhydrous magnesium sulfate. Upon concentrating the reaction mixture under reduced pressure, lactione (2 g) was obtain as oil.

Workup

  1. temperatureunder reflux for 2 hours
  2. customas removing water by Dean-Stark trap
  3. customthe reaction
  4. washThe reaction mixture was washed with water and saturated brine sequentially
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationUpon concentrating the reaction mixture under reduced pressure, lactione (2 g)
  7. customwas obtain as oil

Sources & evidence

ORD record
ord-fa5cb4fe39414a9681bb88d928325fba
Source dataset
uspto-grants-2000_03
Patent number
US06034087

Reaction notes

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