1-Decanethiol → HCID 178442874、化合物

In a 3000 ml flask equipped with a stirrer and a condenser were charged 132 g of 11-bromoundecanoic acid, 91.5 g of n-decanthiol, 59.4 g of sodium methoxide (28% methanol solution) and 1500 ml of methanol, and the mixture was refluxed for 12 hours. After completion of the reaction, the reaction mixture was cooled to room temperature, precipitated crystals were collected by filtration under reduced pressure and the resulting crystals were washed with methanol. The resulting crystals were suspended in 5000 ml of distilled water, and the suspension was neutralized by a conc. hydrochloric acid, and the crystals were again collected by filtration under reduced pressure. The crystals were washed with water until the washed solution became neutral, and recrystallized from ethanol to obtain 140.5 g of the title compound.

1. customIn a 3000 ml flask equipped with a stirrer and a condenser
2. temperaturethe mixture was refluxed for 12 hours
3. customAfter completion of the reaction
4. customprecipitated crystals
5. filtrationwere collected by filtration under reduced pressure
6. washthe resulting crystals were washed with methanol
7. filtrationthe crystals were again collected by filtration under reduced pressure
8. washThe crystals were washed with water until the washed solution
9. customrecrystallized from ethanol

ORDレコード

ord-89ee4cff4ea841b6b3a3a1ee7cc50dff

出典データセット

uspto-grants-2001_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06184180B2