Bromoform → HCID 21452187、化合物

cyclotridecanone: 200 ml of a 50 % aqueous solution of NaOH were added dropwise under vigorous stirring to a mixture of 132 g of cyclododecene (CHEMICAL SAMPLE Co - Columbus, Ohio - USA), 600 g of bromoform and 4 g of tetramethylammonium bromide. The mixture was then left at a temperature between 40° and 50° under stirring during 2 h, whereupon it was left at room temperature overnight and diluted with water. Finally the reaction mixture was extracted with 3 fractions of 300 ml each of ether. The combined extracts, after the usual treatments of washing, drying and evaporation, gave a residue which upon fractional distillation under reduced pressure yielded 173 g (92 %) of 2,2-dibromo-bicyclo[10.1.0]tridecane.

1. waitThe mixture was then left at a temperature between 40° and 50°
2. waitwas left at room temperature overnight
3. extractionFinally the reaction mixture was extracted with 3 fractions of 300 ml each of ether
4. washThe combined extracts, after the usual treatments of washing
5. customdrying
6. customevaporation
7. customgave a residue which
8. distillationupon fractional distillation under reduced pressure

ORDレコード

ord-50b3cba028d0444e8df9b173bc48c74d

出典データセット

uspto-grants-1977_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04009127