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Tetrahydrofuran → 4-[[Bis(p-dimethylaminophenyl)methoxy]acetyl]Morpholine
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 | 1,1,3,3-Tetramethylguanidine | HCID 66460 | — |
| 反応物 | 4,4'-Bis(dimethylamino)benzhydrol | HCID 92742 | — |
| 触媒 | Methanesulfonic Acid | HCID 6395 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 4-[[Bis(p-dimethylaminophenyl)methoxy]acetyl]Morpholine | HCID 20488036 | — |
反応手順
A solution of 4,4'-bis(N,N-dimethylamino)benzhydrol, methyl ether (9.0 g, 0.032 mole), glycol morpholinamide (4.6 g, 0.032 mole), 150 ml of tetrahydrofuran, 250 ml of n-hexane and 4 drops of methanesulfonic acid was refluxed for about 8 hours, during which time an additional 200 ml of solvent was added. The volume was reduced to 200 ml and the color was discharged with tetramethylguanidine. The solution was filtered hot and then cooled to precipitate a white solid. The solid was recrystallized from 350 ml of methyl cyclohexane to give 4.9 g of blue crystals; mp 147.8°-150° 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-aedb3f7bf82141bca0c692617ca9a875 |
| 出典メモ | uspto-grants-1982_08 |