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Tetrahydrofuran → Bis(p-dimethylaminophenyl)Methoxy Acetic Acid, Benzyl Ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Dimethyl Ether | HCID 8254 | — |
| 反応物 | 4,4'-Bis(dimethylamino)benzhydrol | HCID 92742 | — |
| 反応物 | Benzyl 2-hydroxyacetate | HCID 561337 | — |
| 触媒 | Methanesulfonic Acid | HCID 6395 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | Bis(p-dimethylaminophenyl)Methoxy Acetic Acid, Benzyl Ester | HCID 131712798 | — |
反応手順
A solution of 4,4'-bis(N,N-dimethylamino)benzhydrol, methyl ether (11.0 g, 0.039 mole), benzyl glycolate (6.6 g, 0.039 mole), 90 ml of tetrahydrofuran, 200 ml of hexane, and 10 drops of methanesulfonic acid was refluxed for 6 hours, replacing solvent as distillate was removed; then, 10 drops of tetramethylguanidine was added to discharge the color and the reaction mixture was filtered hot and cooled. A white solid formed which was filtered, washed with petroleum ether and then recrystallized from 4/1 hexane/acetone. The resulting white crystalline product had a mp 101.8°-103° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04343939 |
| 出典データセット | uspto-grants-1982_08 |
| ORD ID | ord-c8c7ee5975cb486097236de1755ecc83 |
| 出典メモ | uspto-grants-1982_08 |