関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,2-Ethanedithiol | HCID 10902 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | Methyl 3-chloro-4-cyano-2-methylbenzoate | HCID 68579417 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Chloro-4-(hydroxymethyl)-3-methylbenzonitrile | HCID 68577571 | 66.5% |
反応手順
To a pressure reaction flask containing compound 7A (1.5 g, 7.2 mmol) in THF (30 mL) were added 1,2-ethanedithiol (2.4 g, 28.6 mmol) and NaBH4 (812 mg, 21.5 mmol). It was sealed, and heated at 70° C. for 2 hr, and cooled to RT. The reaction mixture was concentrated, dissolved in EtOAc, washed with water, dried over Na2SO4, and concentrated. Recrystallization in EtOAc/hexanes give the title compound (870 mg). (ES) m/z 182 [M+H]+; 204 [M+Na]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07696241B2 |
|---|
| 出典データセット | uspto-grants-2010_04 |
|---|
| ORD ID | ord-6f973348b7b245bc91aa790a6ac3c759 |
|---|
| 出典メモ | uspto-grants-2010_04 |
|---|
