関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Adamantanecarboxylic acid | HCID 13235 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 3-Bromoadamantane-1-carboxylic acid | HCID 30818 | 75.7% |
反応手順
More specifically, adamantane-1-carboxylic acid (1) (45 g, 0.25 mol) was added to mixture of AlCl3 (45 g, 0.34 mol) and Br2 (450 g) at 0° C. and stirred at 0-10° C. for 48 hrs, kept 5 hrs at about 20° C., poured on to 500 g crushed ice, diluted with 300 ml CHCl3 and decolorized with solid Na2S2O5. The aqueous phase was extracted with Et2O (50 ml×2). The combined organic solution was washed with H2O and extracted with 10% NaOH. The alkaline extraction was acidified with 2N H2SO4 and provided 49 g (yield=75.7%) of 3-bromo-adamantane-1-carboxylic acid (2).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08557800B2 |
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| 出典データセット | uspto-grants-2013_10 |
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| ORD ID | ord-7ecb62d5996541fa92488b9dc2f5d27f |
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| 出典メモ | uspto-grants-2013_10 |
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