Lithium → HCID 178500586, compound

HRID 1759165Notes

Reaction equation

HRID 1759165 reaction equation
C[O:2][CH2:3][PH:4]([C:6](=[O:13])[CH2:7][CH2:8][C:9]([O:11][CH3:12])=[O:10])=[O:5].[Li:14]>[I-].[Li+].C(C(C)=O)C(C)C>[Li:14].[OH:2][CH2:3][PH:4]([C:6](=[O:13])[CH2:7][CH2:8][C:9]([O:11][CH3:12])=[O:10])=[O:5]

Participants

5

Reactant 2

HCID 3028194LithiumHCID 178502583HCID 178502583, compound

Product 1

HCID 178500586HCID 178500586, compound

Reagents, catalysts & solvents 2

HCID 7909Methyl Isobutyl KetoneSolventHCID 66321Lithium iodideSolvent

Procedure

The product of step (a) (16.0 g) was dissolved in a 0.5 M solution of anhydrous lithium iodide in methyl isobutyl ketone (170 ml) and the solution heated under reflux with stirring for 2 hours. After cooling the crude lithium salt was filtered off, washed with acetone and dried. The product (12.0 g) was dissolved in methanol (50 ml) and diluted with acetone (500 ml). The precipitated impurities were filtered off and the filtrate was evaporated to dryness to give the title product as a deliquescent, pale yellow solid (9.5 g). The salt has no sharp melting point and gradually softens and decomposes above 195° C. Elemental analysis indicates the monohydrate:

Workup

  1. temperaturethe solution heated
  2. temperatureunder reflux
  3. filtrationwas filtered off
  4. washwashed with acetone
  5. customdried
  6. dissolutionThe product (12.0 g) was dissolved in methanol (50 ml)
  7. additiondiluted with acetone (500 ml)
  8. filtrationThe precipitated impurities were filtered off
  9. customthe filtrate was evaporated to dryness

Sources & evidence

ORD record
ord-0c563c2f43994ce3b441cd8739bd3620
Source dataset
uspto-grants-1982_07
Patent number
US04339443

Reaction notes

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