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Ethyl Acetate → 1-Phenylethanethiol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | S-(1-phenylethyl) ethanethioate | HCID 11126866 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | tert-Butyl methyl ether | HCID 15413 | — |
| 生成物 | 1-Phenylethanethiol | HCID 141850 | 99.3% |
反応手順
In a synthesis carried out according to Hoppe, et al., Angew. Chem. Int. Ed., 36(24), 2784 (1997), at room temperature, 2.1 g of lithium aluminum hydride and 100 mL of methyl tertiary butyl ether are added to a 250 mL round-bottom flask. To this suspension 18 g of thioacetic acid S-(1-phenyl-ethyl)ester in 50 mL MTBE is added. The mixture is stirred for 15 h at room temperature. 5 mL of ethyl acetate and 2.5 mL of sodium hydroxide (1 M in water) are added. The reaction mixture is filtered over a sodium sulphate plug. The filtrate is concentrated to give 13.7 g of a yellow liquid which is purified by distillation.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07585535B2 |
| 出典データセット | uspto-grants-2009_09 |
| ORD ID | ord-3d4653a7fcd448f080fec43de29e6741 |
| 出典メモ | uspto-grants-2009_09 |