関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | Phenyl chloroformate | HCID 15891 | — |
| 反応物 | 3-Methyl-3-oxetanemethanol | HCID 137837 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-Phenyloxycarbonyloxymethyl-3-methyloxetane | HCID 18939770 | — |
反応手順
A 0.552 mL (4.42 mmol) sample of phenoxycarbonylchloride in 2 mL of methylene chloride was added to a solution of 376 mg (3.68 mmol) of 3-hydroxymethyl-3-methyloxetane and 60.7 mL (5.52 mmol) of 4-methylmorpholine in 2 mL of methylene chloride cooled in an ice bath. The mixture was stirred at 0° C. for 3.5 hours. The mixture was diluted with methylene chloride, which was washed with water, dried and concentrated. The crude product was chromatographed on silica gel, eluting with 20% ethyl acetate in hexane. The solvent was removed and the product dried to afford 0.582 g of the title compound, which was taken directly to the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05616714 |
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| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-8aae3345647e4549a583ae68af8ea5d0 |
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| 出典メモ | uspto-grants-1997_04 |
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