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Formic Acid → [Benzenesulfonyl-(4-cyano-2-methylsulfanyl-phenyl)-methyl]-carbamic acid tert-butyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formic Acid | HCID 284 | — |
| 反応物 | tert-Butyl carbamate | HCID 77922 | — |
| 反応物 | Benzenesulfinic acid, sodium salt | HCID 2723840 | — |
| 反応物 | 4-Formyl-3-(methylsulfanyl)benzonitrile | HCID 58133742 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | [Benzenesulfonyl-(4-cyano-2-methylsulfanyl-phenyl)-methyl]-carbamic acid tert-butyl ester | HCID 118692905 | — |
反応手順
Formic acid (3.0 mL, 79 mmol) is added to a solution of tert-butyl carbamate (1.436 g, 12.3 mmol), 4-formyl-3-methylsulfanyl-benzonitrile (INTERMEDIATE 1; 1.975 g, 11.1 mmol) and sodium benzenesulfinate (2.012 g, 12.2 mmol) in a mixture of THF (3.0 mL) and water (7 mL), and the mixture is stirred at room temperature for 3 days. Water is added, the precipitate is filtered off and washed with water. The precipitate is treated with tert-butyl methyl ether, and the mixture is stirred for 30 min. The precipitate is filtered off, washed with tert-butyl methyl ether and dried. Yield: 3.5 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09440930B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-69decbb807f24d3d9db94a2635fc07e2 |
| 出典メモ | uspto-grants-2016_09 |