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Acetic Acid → 3-Methyl-2-oxooct-6-inylphosphonic acid dimethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Methylphosphonic acid | HCID 13818 | — |
| 反応物 | 2-Methylhept-5-ynoic acid ethyl ester | HCID 53691389 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 3-Methyl-2-oxooct-6-inylphosphonic acid dimethyl ester | HCID 53860064 | — |
反応手順
At -70° C., 73 ml of a 1.7-molar butyllithium solution in hexane is added dropwise to a solution of 18.6 g of the dimethyl ester of methanephosphonic acid in 280 ml of tetrahydrofuran; the mixture is stirred for 15 minutes and a solution of 10.5 g of 2-methylhept-5-ynoic acid ethyl ester in 48 ml of tetrahydrofuran is gradually added thereto. The mixture is stirred for 4 hours at -70° C., neutralized with acetic acid, and evaporated under vacuum. The distillation of the residue under vacuum at 0.6 torr and 130° C. yields 10.8 g of the title compound as a colorless fluid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04423067 |
| 出典データセット | uspto-grants-1983_12 |
| ORD ID | ord-1f1123aa3c8649288837c9d8507ab92f |
| 出典メモ | uspto-grants-1983_12 |