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Hydrochloric Acid → 2-Methyl-1,2-oxaphospholane 2-oxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Methacrylic Acid | HCID 4093 | — |
| 反応物 | Methyl phosphonous dichloride | HCID 61194 | — |
| 反応物 | (3-Hydroxypropyl)methylphosphinic acid | HCID 20291967 | — |
| 生成物 | 2-Methyl-1,2-oxaphospholane 2-oxide | HCID 104467 | — |
| 生成物 | 2,4-Dimethyl-2,5-dioxo-1,2-oxa-phospholane | HCID 20392213 | — |
反応手順
A mixture of 43 g (0.5 mole) of methacrylic acid and 69 g (0.5 mole) of 3-hydroxypropyl-methyl-phosphinic acid is added to 58.5 g (0.5 mole) of methyldichloro-phosphine at 50°-60° C., while hydrogen chloride is discharged. Subsequently heating takes place under water jet vacuum to an internal temperature of up to 150° C. The residue is distilled under reduced pressure. 35 g of 2-methyl-2-oxo-1,2-oxa-phospholane (boiling point at 1.5 mm Hg: 120°-130° C.) and 55 g of 2,4-dimethyl-2,5-dioxo-1,2-oxa-phospholane (boiling point at 0.7 mm Hg: 150°-155° C.) are obtained. The yield in 2,4-dimethyl-2,5-dioxo-1,2-oxa-phospholane represents 71% of the theoretical yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04138433 |
| 出典データセット | uspto-grants-1979_02 |
| ORD ID | ord-6af611a28fe749208ba3246bd685bf5f |
| 出典メモ | uspto-grants-1979_02 |