化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → 2,6-Dimethyl-3-(2-chloroethyl)-5,6-dihydro-1,4-oxathiin
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3,5-Dichloropentan-2-one | HCID 94032 | — |
| 反応物 | 1-Mercapto-2-propanol | HCID 102545 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2,6-Dimethyl-3-(2-chloroethyl)-5,6-dihydro-1,4-oxathiin | HCID 14551707 | 47% |
反応手順
A mixture of 0.1 mole (15.4 g.) 3,5-dichloro-2-pentanone, and 0.1 mole (9.2 g.) 1-mercapto-2-propanol was stirred in 100 ml toluene; 0.1 mole (10.4 g.) triethylamine was added dropwise. The mixture was stirred at room temperature overnight, then washed with dilute hydrochloric acid and reluxed with 0.5 g. PTSA, using a Dean-Stark trap to remove water for about 7 hours. The PTSA solution was washed with sodium bicarbonate, dried over magnesium sulfate and the solvent was removed. The product was distilled; bp 80°-82°/0.1 mm. Yield 47%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04822813 |
| 出典データセット | uspto-grants-1989_04 |
| ORD ID | ord-a365ace1836d41c4a549625275e951ff |
| 出典メモ | uspto-grants-1989_04 |