HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 6-Methyl-1,3-benzoxazole-2-thiol
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | 2-Amino-5-methylphenol | HCID 76082 | — |
| Edukt | Potassium ethylxanthate | HCID 2735045 | — |
| Lösungsmittel | Pyridine | HCID 1049 | — |
| Produkt | 6-Methyl-1,3-benzoxazole-2-thiol | HCID 963501 | — |
Reaktionsschritte
Step 1 A mixture of 6-amino-m-cresol (593.7 mg, 4.82 mmol) and potassium O-ethyl xanthate (850 mg, 5.30 mmol) in pyridine (10 mL) was stirred and heated to reflux for 2 h. It was cooled to rt, poured into a mixture of ice-water (40 mL), and concentrated HCl (4 mL). The solid was collected, washed with water, and dried in the hood overnight and then in a vacuum oven at 45° C. for 3 h. The product 6-methyl-1,3-benzoxazole-2(3H)-thione was obtained as beige powder (735 mg, yield 92.3%). 1H NMR (300 MHz, DMSO-d6) δ 7.10 (s, 1H), 7.03 (d, 2H), 2.42 (s, 3H); LC-MS ret. time 2.37 min (method 2), m/z 166.0 (MH+).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07423156B2 |
| Quelldatensatz | uspto-grants-2008_09 |
| ORD ID | ord-c6f9766480144aaa9938e5f6d6eb0e29 |
| Quellennotiz | uspto-grants-2008_09 |