
4-nitro-1,3-benzoxazole-2-thiol synthesis
- Product Name:4-nitro-1,3-benzoxazole-2-thiol
- CAS Number:101495-34-5
- Molecular formula:C7H4N2O3S
- Molecular Weight:196.18
Yield:101495-34-5 79%
Reaction Conditions:
Stage #1: carbon disulfide;2-Amino-3-nitrophenolwith potassium hydroxide in ethanol;water;Heating / reflux;
Stage #2: with hydrogenchloride;water in ethanol;
Steps:
6
EXAMPLE 6 Preparation of 4-Nitro-3H-benzoxazole-2-thione A solution of KOH (3.31 g, 59.0 mmol) in EtOH and water was treated with carbon disulfide (10.4 g, 136.3 mmol) followed by 2-amino-3-nitrophenol (7.00 g, 45.4 mmol). The mixture was heated at reflux temperature overnight, cooled, concentrated, acidified with 1M HCl and filtered. The filtercake was washed with water and dried in vacuo to provide the title compound (7.0 g, 79%), characterized by NMR and mass spectral analyses.
References:
US2007/281945,2007,A1 Location in patent:Page/Page column 11