関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1,3-Benzenedisulfonyl dichloride | HCID 96240 | — |
| 反応物 | HCID 20574811 | HCID 20574811 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 54391157 | HCID 54391157 | 100.1% |
反応手順
To a stirred solution of 6-t-butyl-3-(butylaminomethyl)-2,4-dimethylphenol (5.26 grams; 0.02 mole) in acetone (40 mls) is slowly added 1,3-benzenedisulfonyl chloride (2.75 grams; 0.01 mole) while maintaining the temperature at 25°-30° C. by cooling. To this mixture is slowly added a solution of 50% caustic soda (1.6 grams; 0.02 mole) in water (22 mls) while maintaining the temperature at 25°-30° C. by cooling. The mixture is allowed to come to room temperature and stirred for 15 hours. The mixture is then allowed to settle, and the upper layer is separated and slowly treated with ice water (100 mls). The resulting oil which separates solidifies upon standing for 2.5 hours. The solid is then recovered by filtration to obtain the crude product (7.3 grams; 100% of theoretical). Recrystallization of the crude product from glacial acetic acid affords the pure product (2.5 grams; m.p. 143°-144.5° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04278577 |
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| 出典データセット | uspto-grants-1981_07 |
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| ORD ID | ord-939760b5f2914b99835e6e0774665500 |
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| 出典メモ | uspto-grants-1981_07 |
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