FIELD: chemistry.
SUBSTANCE: as a reducer applied is diisobutylaluminiumhydride (DIBAH), taken in a molar ratio of verbenone: DIBAH, equal to 1:1.8-2.2, and as organic solvent - dichloromethane, the process is carried out at temperatures of minus 78°C - minus 65°C for 90-120 min, and separation of the target product is carried out by processing a reaction mixture with water, taken in a quantity of 300-400% of a stoichiometrically necessary one for decomposition of DIBAG excess, separation of sediment and its washing with dichloromethane, removal of water remains from the filtrate above sodium sulphate and evaporation of an organic solvent under reduced pressure.
EFFECT: method makes it possible to increase stereo-selectivity of the reaction and increase the output of the target product.
1 tbl
Title | Year | Author | Number |
---|---|---|---|
METHOD OF SYNTHESIS OF CIS-VERBENOL | 2001 |
|
RU2189967C1 |
VERBENONE PREPARATION METHOD | 2003 |
|
RU2250208C2 |
CIS/TRANS-CITRAL AND (ISO)PIPERITONOLE PROCESS | 2008 |
|
RU2357949C1 |
OCTAFLUORO-2-BUTENE SYNTHESIS PROCESS | 2022 |
|
RU2794898C1 |
METHOD FOR PREPARING TRANS-PINENYL SULFIDES | 2005 |
|
RU2296749C1 |
PROCESS FOR PREPARING 3-PHENOXYBENZYL ALCOHOL | 0 |
|
SU1097600A1 |
METHOD FOR SYNTHESIS OF 2-HYDROXY-6-ISOPROPENYL-3-METHYL-CYCLOHEX-3-ENONE | 2009 |
|
RU2409549C1 |
METHOD OF PRODUCING 3α-HYDROXY-10β-PINANONE-4 | 2012 |
|
RU2509073C1 |
CATALYST SYSTEM FOR PRODUCTION OF CONJUGATED DIENE/MONOOLEFIN COPOLYMERS AND SAID COPOLYMERS | 2004 |
|
RU2400492C2 |
METHOD FOR PREPARING VERBENOL AND ALPHA-PINENE EPOXIDE | 2003 |
|
RU2235712C1 |
Authors
Dates
2014-10-20—Published
2013-04-24—Filed