関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | tert-Butyl mercaptan | HCID 6387 | — |
| 反応物 | 3-Amino-4-methylbenzoic acid | HCID 75568 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178425897 | HCID 178425897 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07176242B2 |
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| 出典データセット | uspto-grants-2007_02 |
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| ORD ID | ord-3633e92ea72043d4817cd4bbe11f5cd9 |
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| 出典メモ | uspto-grants-2007_02 |
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