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Hydrochloric Acid → 5-(4-Chloro-3-chlorosulfonylphenyl)-5-hydroxy-1-methyl-2-pyrrolidone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sulfur Dioxide | HCID 1119 | — |
| 反応物 | 5-(3-Amino-4-chlorophenyl)-5-hydroxy-1-methylpyrrolidin-2-one | HCID 14256803 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 触媒 | Cupric chloride dihydrate | HCID 61482 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-(4-Chloro-3-chlorosulfonylphenyl)-5-hydroxy-1-methyl-2-pyrrolidone | HCID 14256804 | — |
反応手順
A solution of 9.9 g of sodium nitrite in 60 ml of water is metered into, below the surface of, a solution of 30.5 g of 5-(3-amino-4-chlorophenyl)-5-hydroxy-1-methyl-2-pyrrolidone in 300 ml of half-concentrated hydrochloric acid at at 0° to 5° C. The reaction mixture is stirred while cooling for a further 10 min, and then a mixture of 15.2 g of copper(II)chloride dihydrate and 450 ml of a saturated solution of sulfur dioxide in glacial acetic acid is added in portions. The mixture is stirred for a further 30 min, and then the sulfonyl chloride is precipitated by addition of water, and the crystals are filtered off. Melting point 137°-139° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04849444 |
| 出典データセット | uspto-grants-1989_07 |
| ORD ID | ord-d3003e71854a4252b620381bf1185b50 |
| 出典メモ | uspto-grants-1989_07 |