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Triethylamine → HCID 86753273、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1,3-Cyclopentanedicarboxylic anhydride | HCID 239799 | — |
| 反応物 | N-(Benzyloxy)-1-phenylmethanamine--hydrogen chloride (1/1) | HCID 18358890 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 86753273 | HCID 86753273 | — |
反応手順
552 mg of 3-Oxabicyclo[3.2.1]octane-2,4-dione (3.94 mmol, prepared according to the procedure described in Chem. Lett., p 93, (1994)) is added to a rapidly stirring solution of triethylamine (0.55 mL, 3.94 mmol) and N-benzyl-O-benzylhydroxylamine hydrochloride (983 mg, 3.94 mmol) in CH2Cl2 in a flame dried flask under nitrogen. After stirring at ambient temperature for 3 days, the reaction is quenched with aqueous citric acid (1M). Extraction into CH2Cl2 (3×50 mL), followed by drying over MgSO4, yielded a pale yellow oil, 1.51 g. Recrystallization in ethyl acetate/hexane provided the product as a white crystalline solid, 1.32 g (95%). mp. 118°-120° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05830869 |
| 出典データセット | uspto-grants-1998_11 |
| ORD ID | ord-a9acd726059349c9be9f4de5bfaaf32b |
| 出典メモ | uspto-grants-1998_11 |