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Trimethyl phosphite → [2-Fluoro-1,3-phenylenebis(methylene)]bisphosphonic acid tetramethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trimethyl phosphite | HCID 8472 | — |
| 反応物 | 1,3-Bis(bromomethyl)-2-fluorobenzene | HCID 2736003 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | [2-Fluoro-1,3-phenylenebis(methylene)]bisphosphonic acid tetramethyl ester | HCID 86747693 | — |
反応手順
A solution of 2,6-bis(bromomethyl)-1-fluorobenzene (2.82 g, 0.010 mole) and trimethylphosphite (5.0 mL, 0.042 mole) in toluene (25 mL) is heated at reflux temperature for 24 hours, after which the solvent and excess trimethylphosphite are removed under reduced pressure. The solid residue is crystallized from ethyl acetate-hexane, giving 3.12 g (0.0089 mole, 89%) of of the title compound, mp 116.5°-117.5° C. Recrystallization gives 2.64 g, mp 117°-118° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05298498 |
| 出典データセット | uspto-grants-1994_03 |
| ORD ID | ord-fd7c419735424e3d905e0ec459d98bd1 |
| 出典メモ | uspto-grants-1994_03 |