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Dimethylamine, hydrochloride → 2-Amino-4-chloromethyl-6-dimethylaminopyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylamine, hydrochloride | HCID 10473 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | 4-Chloro-6-(chloromethyl)pyrimidin-2-amine | HCID 20153488 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-Amino-4-chloromethyl-6-dimethylaminopyrimidine | HCID 20153502 | — |
反応手順
8.1 Parts of dimethylamine hydrochloride was added to a solution of 2.3 parts of sodium in 20 parts of methanol. The resulting mixture was added dropwise with stirring over about 10 minutes to a solution of 9.9 parts of 2-amino-4-chloro-6-chloromethylpyrimidine in 50 parts of methanol. The reaction was monitored by TLC and when reaction was complete the solvent was evaporated and the residue stirred with about 20 parts of water. The solid obtained was filtered and dried. The product was purified by chromatography on silica, eluted with ethyl acetate, followed by sublimation at 110° C./0.04 mb to give 2-amino-4-chloromethyl-6-dimethylaminopyrimidine m.p. 127°-129° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04723006 |
| 出典データセット | uspto-grants-1988_02 |
| ORD ID | ord-49bd71cf48ae45fcbb90a9526cdec8dd |
| 出典メモ | uspto-grants-1988_02 |