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Chloroacetonitrile → (4-(4-(Methylsulfonyl)phenoxy)phenoxy)acetonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloroacetonitrile | HCID 7856 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Phenol, 4-(4-(methylsulfonyl)phenoxy)- | HCID 514882 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | (4-(4-(Methylsulfonyl)phenoxy)phenoxy)acetonitrile | HCID 13078520 | 92.4% |
反応手順
To a solution of 5.29 g (0.0200 mole) of 4-(4-(methylsulfonyl)phenoxy)phenol and 1.51 g (0.0200 mole) of 2-chloroacetonitrile in 100 ml of acetonitrile was added 3.0 g (0.0220 mole) of K2CO3. The mixture was heated at reflux for 3.5 hrs and cooled. The mixture was poured into aqueous NaOH and the product extracted from the mixture with CH2Cl2. The organic layer was extracted with aqueous NaOH, water and dried (Na2SO4). Removal of solvent in vacuo afforded 5.6 g (92.4% yield) of product. Recrystallization from ethanol followed by washing with aqueous NaOH and water afforded purified (4-(4-(methylsulfonyl)phenoxy)phenoxy)acetonitrile, mp 114°-115.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04505929 |
| 出典データセット | uspto-grants-1985_03 |
| ORD ID | ord-36a243dff25145769df82ed4d451001c |
| 出典メモ | uspto-grants-1985_03 |