Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | tert-Butyl mercaptan | HCID 6387 | — |
| Edukt | 3-Amino-4-methylbenzoic acid | HCID 75568 | — |
| Edukt | Sodium Acetate | HCID 517045 | — |
| Edukt | Sodium Nitrite | HCID 23668193 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | HCID 178425897 | HCID 178425897 | — |
Reaktionsschritte
To a mixture of 3-amino-4-methyl benzoic acid (5.0 g) in water (50 mL) was added concentrated hydrochloric acid (15 mL). The mixture was chilled to 0° C. in an ice/acetone bath. Sodium nitrite (2.28 g) was dissolved in water (10 mL) and slowly added to the mixture at 0° C. The pH was adjusted to 6 with saturated sodium acetate and 2-methyl-2-propanethiol (1.8 mL) was added. The mixture was stirred for 1 h and the resulting solids were collected by filtration, washed with water and dried under reduced pressure to give 5.7 g of the title compound: 1H NMR (CDCl3) δ 1.61, 2.20, 7.38, 7.55, 9.67.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07727997B2 |
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| Quelldatensatz | uspto-grants-2010_06 |
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| ORD ID | ord-d460acee005d487d96d6209089279d3e |
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| Quellennotiz | uspto-grants-2010_06 |
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