関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 6-Diazo-5,6-dihydro-5-oxo-1-naphthalenesulfonyl chloride | HCID 136378771 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4,7-Methano-1H-indene, octahydro- | HCID 17795 | 88.5% |
反応手順
To a solution of 1.86 g 4,8-Bis(hydroxyeth-1'-yl)tricyclo [5.2.1.02,6 ] decane, 0.93 g of 4-di-methylamino-pyridine, 4.7 ml of triethylamine and 30 ml of CH2Cl2 at 0° C. was added a solution of 7.8 g of 6-diazo-5,6-dihydro-5-oxo-1-naphthalene sulfonyl chloride and 80 ml of methylene chloride over 0.5 hr. The mixture was stirred 1/2 hour at 9° C. and 6 hours at 25° C. and then diluted with 100 ml of methylene chloride. The mixture was then filtered and the methylene chloride phase washed with 100 ml of 10% sodium bicarbonate solution, 100 ml of water, 100 ml of 2 N sulfuric acid solution 50 ml of 5% sodium bicarbonate solution and 50 ml of water. The solution was then dried over sodium sulfate and the solvent removed at reduced pressure to give 3.5 g of product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04397937 |
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| 出典データセット | uspto-grants-1983_08 |
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| ORD ID | ord-c30b13df8d8d43868ce742d1f051f00a |
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| 出典メモ | uspto-grants-1983_08 |
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