関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Trityl chloride | HCID 6456 | — |
| 反応物 | 2-Bromoethylamine hydrobromide | HCID 2774217 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | (2-Bromoethyl)tritylamine | HCID 15718287 | — |
反応手順
272.1 g (976 mmol) of triphenylchloromethane, 800 ml of dichloromethane and 200 g (976 mmol) of 2-bromoethanamine hydrobromide are introduced into a 2-1 round bottom flask placed under nitrogen. The mixture is stirred and 300 ml of triethylamine are added dropwise and stirring is continued for 48 h. The triethylamine hydrochloride which precipitates is separated off, water is added to the filtrate, the organic phase is separated off and is washed with water and dried over sodium sulphate, and the solvent is evaporated off. An oil is obtained, which is purified by chromatography on a column of silica gel. After recrystallisation from a mixture of dichloromethane and cyclohexane 273.17 g of white solid are obtained. Melting point: 108°-109° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05164397 |
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| 出典データセット | uspto-grants-1992_11 |
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| ORD ID | ord-276a018d26c74d3d84d0e19d06915cf1 |
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| 出典メモ | uspto-grants-1992_11 |
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