関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | 1-Chloroethyl chloroformate | HCID 521305 | — |
| 反応物 | 3-(Benzyloxy)-1-(diphenylmethyl)azetidine | HCID 16089448 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-(Benzyloxy)azetidine hydrochloride | HCID 46737011 | 92% |
反応手順
A 16 mL vial was charged with 3-(benzyloxy)-1-(diphenylmethyl)azetidine (103 mg, 0.31 mmol; which may be prepared as described in Step 1) and 1,2-dichloroethane (1.4 mL). 1-Chloroethyl chloroformate (45 μL, 0.41 mmol) was added and the reaction mixture was stirred at 70° C. for 1.5 h. After cooling to room temperature, methanol (1.4 mL) was added and the reaction mixture was stirred at 70° C. for 1.5 h. The reaction mixture was cooled and concentrated to dryness. The residue was purified on column chromatography (eluent: Pentane/NH3 7N in MeOH, 98/2) to give the title compound (57 mg, 92%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09051321B2 |
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| 出典データセット | uspto-grants-2015_06 |
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| ORD ID | ord-60d5d5d6edc7453e87e9a8b5d20feb7b |
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| 出典メモ | uspto-grants-2015_06 |
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