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Methanol → 2-(4-Chlorobutyl)-1,3-dithiane-2-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Lithium Hydroxide | HCID 3939 | — |
| 反応物 | Ethyl 2-(4-chlorobutyl)-1,3-dithiane-2-carboxylate | HCID 86649922 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(4-Chlorobutyl)-1,3-dithiane-2-carboxylic acid | HCID 58110016 | 81% |
反応手順
Step AS (2): To a solution of ethyl 2-(4-chlorobutyl)-1,3-dithiane-2-carboxylate (550 mg, 1.94 mmol) in THF (5 mL) was added a solution of LiOH (233 mg, 9.72 mmol) in water (2 mL). Methanol (2 mL) was added and the resulting mixture was stirred at rt for 2 d. The solvents were removed in vacuo. Aqueous 1 N HCl (50 mL) was added. The mixture was extracted with EtOAc (80 mL). The organic layer was washed with water, dried over sodium sulfate, filter, and concentrated in vacuo to afford 2-(4-chlorobutyl)-1,3-dithiane-2-carboxylic acid (400 mg, 1.57 mmol, 81% yield). LC-MS (M+H)+ 253.0. The crude product was used for subsequent chemistry without purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08349880B2 |
| 出典データセット | uspto-grants-2013_01 |
| ORD ID | ord-203d55182dac483797d0336629fe16b8 |
| 出典メモ | uspto-grants-2013_01 |