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Lithium diisobutylaluminum hydride → HCID 69666864、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Lithium diisobutylaluminum hydride | HCID 22042274 | — |
| 反応物 | Methyl 3-(chloromethylene)-2,3-dihydro-1-benzoxepin-7-carboxylate | HCID 69667024 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 69666864 | HCID 69666864 | 108.9% |
反応手順
2.72 ml (2.72 mmol) of a lithium diisobutylaluminum hydride solution are added at a temperature of −78° C. to 217 mg (0.87 mmol) of methyl 3-(chloromethylene)-2,3-dihydro-1-benzoxepin-7-carboxylate, prepared according to example 32, in solution in 10 ml of dichloromethane. The solution is stirred at this temperature for 1 hour. A conventional treatment makes it possible to isolate 211 mg (100%) of [3-(chloromethylene)-2,3-dihydro-1-benzoxepin-7-yl]methanol in the form of a white solid comprising two Z/E isomers as a mixture in a 90/10 ratio; 1H NMR (C6D6): 6.98 (d, J=8.2 Hz, 1H), 6.97 (m, 1H), 6.90 (dd, J=8.2 Hz and 2.2 Hz, 1H), 6.07 (d, J=11.8 Hz, 1H), 5.86 (d, J=11.8 Hz, 1H), 5.74 (s, 1H), 4.68 (s, 2H), 4.28 (4.1) (s, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07071340B2 |
| 出典データセット | uspto-grants-2006_07 |
| ORD ID | ord-aafb996dd83d4cf1a59f6366ed0cb2bc |
| 出典メモ | uspto-grants-2006_07 |