化工社化工社 化学情報印刷レポート · 研究参考用
Water → 6-chloro-3-chloromethyl-3H-oxazolo[4,5-b]pyridin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 6-Chloro-3-(hydroxymethyl)oxazolo(4,5-b)pyridin-2(3H)-one | HCID 21426072 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 6-chloro-3-chloromethyl-3H-oxazolo[4,5-b]pyridin-2-one | HCID 21426073 | 83% |
反応手順
39 Parts of thionyl chloride are added dropwise, in a manner ensuring that the internal temperature does not exceed 50° C., to a solution of 45 parts of 3-hydroxymethyl-6-chloro-oxazolo[4,5-b]pyridin-2-(3H)-one in 200 parts of toluene; and the whole is stirred for a further 4 hours at 40°-50° C. The resulting solution is subsequently freed from gases in a water-jet vacuum, and sufficient toluene is evaporated off to leave a crystal sludge that can still just be stirred. After the addition of 100 parts of hexane, filtration is carried out and the filter cake is washed twice with cold hexane. There are obtained 40 parts of 3-chloromethyl-6-chloro-oxazolo[4,5-b]pyridin-2-(3H)-one (83% of theory), m.p. 105°-107° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04033975 |
| 出典データセット | uspto-grants-1977_07 |
| ORD ID | ord-4d64fe1590b54ba38d13df0e6a65285e |
| 出典メモ | uspto-grants-1977_07 |