Acetic Anhydride → HCID 12383395, compound

HRID 1929282Notes

Reaction equation

HRID 1929282 reaction equation
[O:1]1CC[CH2:3][CH2:2]1.C([O-])(O)=O.[Na+].[NH2:11][C:12]1[CH:13]=[C:14]([CH:18]=[CH:19][C:20]=1[Cl:21])[C:15]([OH:17])=[O:16].C(OC(=O)C)(=O)C>C(O)(=O)C>[C:2]([NH:11][C:12]1[CH:13]=[C:14]([CH:18]=[CH:19][C:20]=1[Cl:21])[C:15]([OH:17])=[O:16])(=[O:1])[CH3:3]

Participants

6

Reactant 4

HCID 7918Acetic AnhydrideHCID 8028TetrahydrofuranHCID 760923-Amino-4-chlorobenzoic acidHCID 516892Sodium Bicarbonate

Product 1

HCID 12383395HCID 12383395, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

Tetrahydrofuran (THF) room temperature (RT), NaHCO3 solution 101.9 g (582 mmol) of 3-amino-4-chlorobenzoic acid were suspended in 700 ml of acetic acid and then admixed with 64.8 ml (687 mmol) of acetic anhydride. The mixture was heated under reflux for 15 h and, after cooling, was added to 1.5 l of ice-water. The precipitated crystals were isolated by filtration with suction, washed with water, and dried in a vacuum cabinet at 70° C. for 17 h.

Workup

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 15 h
  3. temperatureafter cooling
  4. customThe precipitated crystals were isolated by filtration with suction
  5. washwashed with water
  6. customdried in a vacuum cabinet at 70° C. for 17 h.

Sources & evidence

ORD record
ord-91e390644c3746869d1e5e9f30e1be62
Source dataset
uspto-grants-2012_05
Patent number
US08188002B2

Reaction notes

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