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Phosphorus oxychloride → 1,4-Ethanonaphthalene, 1,4-dihydro-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 1,4,4a,5,8,8a-Hexahydro-1,4-ethanonaphthalene-5,8-diol | HCID 12657575 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 1,4-Ethanonaphthalene, 1,4-dihydro- | HCID 138994 | 46.8% |
反応手順
To a solution of 27.9 g of tricyclo[6.2.2.02,7]dodeca-4,9-diene-3,6-diol in 165 mL of pyridine were portionwise added 30 mL of POCl3 at 0° C. The reaction was stirred for 3 days at rt before it was quenched by careful addition of ice under cooling. The resulting mixture was extracted with Hept (4×50 mL). The combined organic phases were washed with H2O, 15% HCl solution and again with H2O. The organic phase was dried over MgSO4 and concentrated in vacuo to obtain 10.6 g of the desired compound as yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08314253B2 |
| 出典データセット | uspto-grants-2012_11 |
| ORD ID | ord-4aa477d50f5c4ca08d07c8d4f8a4586d |
| 出典メモ | uspto-grants-2012_11 |