Water → 4-n-Heptyl-4-phenyl-4-silacyclohexane carbaldehyde

12 g of potassium t-butoxide was added to a mixture of 35 g of methoxymethyltriphenylphosphonium chloride and 200 ml of THF to prepare an orange ylide solution. A solution of 28 g of 4-n-heptyl-4-phenyl-4-silacyclohexanone in 50 ml of THF was added to the solution. After agitation for 2 hours at room temperature, the mixture was poured into iced water and extracted with methylene chloride. The extract was washed, dried and concentrated by a usual manner. n-Hexane was added to the resultant concentrate, followed by removal of the resultant triphenylphosphine oxide crystals by filtration. The resultant filtrate was concentrated. The concentrate was hydrolyzed with 100 ml of 20% hydrochloric acid, followed by washing, drying and concentration by a usual manner to obtain 4-n-heptyl-4-phenyl-4-silacyclohexane carbaldehyde.

1. customto prepare an orange ylide solution
2. extractionextracted with methylene chloride
3. washThe extract was washed
4. customdried
5. concentrationconcentrated by a usual manner
6. additionn-Hexane was added to the resultant
7. concentrationconcentrate
8. customfollowed by removal of the resultant triphenylphosphine oxide crystals by filtration
9. concentrationThe resultant filtrate was concentrated
10. washby washing
11. customdrying
12. concentrationconcentration by a usual manner

ORDレコード

ord-185154b6627f4f909d32b9149fae48a3

出典データセット

uspto-grants-1998_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05730901