3-Amino-2-hydroxyacetophenone → HCID 178466153, compound
Reaction equation
[C:1](=S)(OCC)[S-:2].[K+].[CH3:8][C:9]([C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([NH2:17])[C:12]=1[OH:18])=[O:10]>C(O)C>[C:9]([C:11]1[C:12]2[O:18][C:1]([SH:2])=[N:17][C:13]=2[CH:14]=[CH:15][CH:16]=1)(=[O:10])[CH3:8]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
Potassium O-ethyl dithiocarbonate (241 mg, 1.5 mmol) was added to a solution of 3-amino-2-hydroxyacetophenone (113 mg, 0.75 mmol) in ethanol (10 ml) and the mixture was heated to reflux for 16 hours. The reaction was concentrated, water (20 ml) was added thereto and the mixture was adjusted to pH, 3-4 with diluted hydrochloric acid. The separated matter was collected by filtration and dried by heating in vacuo to provide 134 mg (yield 92%) of 7-acetyl-2-mercaptobenzooxazole as a dark solid.
Workup
- temperaturethe mixture was heated
- temperatureto reflux for 16 hours
- concentrationThe reaction was concentrated
- additionwater (20 ml) was added
- filtrationThe separated matter was collected by filtration
- customdried
- temperatureby heating in vacuo
Sources & evidence
- ORD record
- ord-b6a8d26d4bfa43319a5a957d7bc0898e
- Source dataset
- uspto-grants-2005_11
- Patent number
- US06969711B2
Reaction notes
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