Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | 1,3-Benzenedisulfonyl dichloride | HCID 96240 | — |
| Edukt | HCID 20574811 | HCID 20574811 | — |
| Lösungsmittel | Acetone | HCID 180 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | HCID 54391157 | HCID 54391157 | 100,1% |
Reaktionsschritte
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.).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US04278577 |
|---|
| Quelldatensatz | uspto-grants-1981_07 |
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| ORD ID | ord-939760b5f2914b99835e6e0774665500 |
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| Quellennotiz | uspto-grants-1981_07 |
|---|