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Diethyl Ether → 3-Hydroxy-2,2-dimethyl-1-propylthiocyanate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 3-Bromo-2,2-dimethyl-1-propanol | HCID 142501 | — |
| 反応物 | Potassium thiocyanate | HCID 516872 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Hydroxy-2,2-dimethyl-1-propylthiocyanate | HCID 10464453 | 85.4% |
反応手順
A mixture of 16.7 g of 3-bromo-2,2-dimethyl-1-propanol, 14.6 g of potassium thiocyanate and 60 ml of dimethylformamide was stirred for 4 hours at 130°-140° C. The reaction solution was cooled to room temperature (hereinafter means "5°-20° C."), to which a mixture of 200 ml of diethyl ether and 200 ml of water was added. The ethereal layer was collected. The aqueous layer was extracted with 150 ml of diethyl ether. The combined ethereal layers were washed with a saturated saline, dried over anhydrous magnesium sulfate and distilled to remove the solvent. The residue was distilled under reduced pressure to obtain 12.4 g of 3-hydroxy-2,2-dimethyl-1-propylthiocyanate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05155108 |
| 出典データセット | uspto-grants-1992_10 |
| ORD ID | ord-02543adcd5c04215b3f3709bef51e2fd |
| 出典メモ | uspto-grants-1992_10 |