Acetic Anhydride → HCID 12241059, compound

HRID 1287703Notes

Reaction equation

HRID 1287703 reaction equation
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:16][OH:17])=[C:6]([CH:15]=1)[CH:7]([OH:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[C:18](OC(=O)C)(=[O:20])[CH3:19]>C1C=CC=CC=1>[C:18]([O:17][CH2:16][C:5]1[CH:4]=[CH:3][C:2]([Cl:1])=[CH:15][C:6]=1[CH:7]([OH:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)(=[O:20])[CH3:19]

Participants

4

Reactant 2

HCID 7918Acetic AnhydrideHCID 12241058HCID 12241058, compound

Product 1

HCID 12241059HCID 12241059, compound

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent

Procedure

To a solution of 97 g. of the compound of Example 1 in 550 ml. of benzene, 75 ml. of acetic anhydride is added and the mixture is gently refluxed for 3 hours. The cooled solution is washed with aqueous sodium bicarbonate, then with water. The organic phase is dried over sodium sulphate and evaporated to dryness. The residue, after trituration with light petroleum, is crystallized from a mixture of ethyl ether and benzol. M.p. 86°-88° C. Yield 60 g.

Workup

  1. temperaturethe mixture is gently refluxed for 3 hours
  2. washThe cooled solution is washed with aqueous sodium bicarbonate
  3. dry with materialThe organic phase is dried over sodium sulphate
  4. customevaporated to dryness
  5. customThe residue, after trituration with light petroleum, is crystallized from a mixture of ethyl ether and benzol

Sources & evidence

ORD record
ord-ecc95be3887f43128b078849f83f04a2
Source dataset
uspto-grants-1976_10
Patent number
US03985811

Reaction notes

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