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Acetone → HCID 21973119、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | Sodium cyanoborohydride | HCID 5003444 | — |
| 反応物 | 4-((3,5-Bis(trifluoromethyl)benzyloxy)methyl)-4-phenylazepane | HCID 11626160 | — |
| 触媒 | Trifluoroacetic acid | HCID 6422 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 21973119 | HCID 21973119 | 76% |
反応手順
Mixture of isomer A of 4-((3,5-bis(trifluoromethyl)benzyloxy)methyl)-4-phenylazepane (3 mg) and acetone (1.2 mg) in methanol (0.15 mL) was stirred at room temperature for 0.5 hr, then sodium cyanoborohydride (1.0 M solution in THF, 0.02 mL) was added followed by 1 drop of trifluoroacetic acid. The mixture was stirred at 65° C. for overnight and concentrated under vacuum. Then saturated sodium bicarbonate solution and dichloromethane was added to the mixture and the organic layer was separated. The aqueous layer was extracted with dichloromethane 2 times and the combined organic layers were dried over magnesium sulfate, filtered and concentrated under vacuum to give the product as a clear sticky oil (2.5 mg, 76% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07098203B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-c9a402b306ff49baa560b3a2cd76a8ad |
| 出典メモ | uspto-grants-2006_08 |