Acetic Anhydride → HCID 57033109, compound

HRID 2211193Notes

Reaction equation

HRID 2211193 reaction equation
[S:1]([C:5]1[CH:13]=[C:12]([C:14]([OH:16])=[O:15])[CH:11]=[CH:10][C:6]=1[C:7]([OH:9])=[O:8])([OH:4])(=[O:3])=[O:2].C([O:20][C:21](=[O:23])[CH3:22])(=O)C>>[C:21]([C:22]1[CH:11]=[CH:10][C:6]([C:7]([O:8][C:7](=[O:9])[C:6]2[CH:10]=[CH:11][C:12]([C:14]([OH:16])=[O:15])=[CH:13][C:5]=2[S:1]([OH:4])(=[O:3])=[O:2])=[O:8])=[C:5]([S:1]([OH:4])(=[O:3])=[O:2])[CH:13]=1)([OH:20])=[O:23]

Participants

3

Reactant 2

HCID 7918Acetic AnhydrideHCID 98785022-sulfoterephthalic Acid

Product 1

HCID 57033109HCID 57033109, compound

Conditions

Temperature
100 °C

Procedure

A dry 500 ml 3-neck flask was equipped with a condenser, stirrer and thermometer under a nitrogen atmosphere. The vessel was charged with 2-sulfoterephthalic acid (100 g, 447 mmol) and acetic anhydride (127 ml). The solution was stirred at 100° C. for 4 hours and then cooled to room temperature (the reaction mixture became homogeneous at 90° C.). A precipitate which had begun to form at 76° C. was then collected by filtration at room temperature (25° C.) under a N2 atmosphere. It was washed with methylene chloride (5×200 ml) and dried in dessicator under high vacuum for 24 hours. The dry white product melted at 210°-213° C. (Lit 208°-210° C.); 66.8 g (65%).

Workup

  1. customA dry 500 ml 3-neck flask was equipped with a condenser, stirrer
  2. temperaturecooled to room temperature (the reaction mixture
  3. custombecame homogeneous at 90° C.
  4. customto form at 76° C.
  5. filtrationwas then collected by filtration at room temperature (25° C.) under a N2 atmosphere
  6. washIt was washed with methylene chloride (5×200 ml)
  7. customdried in dessicator under high vacuum for 24 hours
  8. customThe dry white product melted at 210°-213° C. (Lit 208°-210° C.)

Sources & evidence

ORD record
ord-b2f94072cc6d4f3f9dbc84c0ad55c01e
Source dataset
uspto-grants-1995_10
Patent number
US05462991

Reaction notes

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