Hydrogen Peroxide → 11-(Methylsulfonyl)peroxyundecanoic acid

温度

40 °C

A stirred mixture of 3 g of 11-(methylsulfonyl)undecanoic acid and 30 mL of methanesulfonic acid was heated to approximately 40° C. The solid dissolved only partially in the methanesulfonic acid at this temperature. Then 1.29 g of 90% hydrogen peroxide was added dropwise. The temperature of the reaction mixture was reduced to room temperature after twenty minutes of reaction time. For the remainder of the two hour reaction time, the reaction mixture was not heated and became homogeneous. The reaction mixture was then cooled in an ice bath forming a solid which was then filtered from solution. The filtrate was poured onto ice prepared from distilled water. A solid formed which was filtered from solution. The two solids collected were combined and washed several times with cold deionized water until the filtrate was no longer strongly acidic. The solid was dried overnight on a watchglass, weighed 2.91 g and had 4.8% by weight active oxygen (84.1% of theoretical).

1. customThe temperature of the reaction mixture was reduced to room temperature after twenty minutes of reaction time
2. customFor the remainder of the two hour reaction time
3. temperaturethe reaction mixture was not heated
4. temperatureThe reaction mixture was then cooled in an ice bath
5. customforming a solid which
6. filtrationwas then filtered from solution
7. additionThe filtrate was poured onto ice
8. customprepared
9. distillationfrom distilled water
10. customA solid formed which
11. filtrationwas filtered from solution
12. customThe two solids collected
13. washwashed several times
14. customThe solid was dried overnight on a watchglass

ORDレコード

ord-e0bec60349e14a77bf99286488f97de3

出典データセット

uspto-grants-1988_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04758369