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2-Amino-4'-chlorobenzophenone → 2-Amino-3-(4-chlorobenzoyl)-alpha-(methylthio)benzeneacetonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Amino-4'-chlorobenzophenone | HCID 76166 | — |
| 反応物 | Methylthioacetonitrile | HCID 99295 | — |
| 反応物 | Tert-Butyl hypochlorite | HCID 521297 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Amino-3-(4-chlorobenzoyl)-alpha-(methylthio)benzeneacetonitrile | HCID 15634730 | 68% |
反応手順
To a solution of 46.3 g (0.2 mole) of 4'-chloro-2-aminobenzophenone and 17.4 g (0.2 mole) of methylthioacetonitrile in 1 liter of methylene dichloride at a temperature of -70° C. was added dropwise 22.2 g (0.21 mole) of tert. butyloxychloride at a rate to ensure that the reaction temperature did not exceed -65° C. The resulting solution was allowed to warm to ambient temperature, washed twice with water, dried over sodium sulphate, and concentrated to give a gum residue. The gum crystallized when it was triturated with diethyl ether. The solid was collected by filtration and recrystallized from 2-propanol to yield 43.0 g (68%) of the title compound as a tan solid, m.p. 122° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04898874 |
| 出典データセット | uspto-grants-1990_02 |
| ORD ID | ord-f7d709ab2e8f43c7bfcb0d3aa454a01a |
| 出典メモ | uspto-grants-1990_02 |