関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Propanoyl bromide, 2-bromo- | HCID 79047 | — |
| 反応物 | 2-Chloro-6-methylbenzylamine | HCID 521799 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | N-(2-bromopropionyl)-2-chloro-6-methylbenzylamine | HCID 21442921 | — |
反応手順
A mixture of 35 parts of 2-chloro-6-methylbenzylamine and 30 parts of triethyl amine in 400 parts of ethylene chloride is stirred and cooled to -35°C. While keeping the temperature between -35° and -20° C., there is added dripwise a solution of 50 parts of 2-bromopropionyl bromide in 160 parts of ethylene chloride. Upon completion, the whole is stirred for one hour at room temperature. The reaction mixture is washed with diluted hydrochloric acid and once with water. The organic phase is dried over magnesium sulfate, filtered and evaporated. The solid residue is crystallized from a mixture of 400 parts of ethanol and 150 parts of water, yielding 40 parts of N-(2-bromopropionyl)-2-chloro-6-methylbenzylamine; mp. 168° -169° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04017631 |
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| 出典データセット | uspto-grants-1977_04 |
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| ORD ID | ord-1b6ce62300c14f95ac4f7a59af9136f3 |
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| 出典メモ | uspto-grants-1977_04 |
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