FIELD: chemistry.
SUBSTANCE: invention pertains to the method of obtaining 7,7-methoxybicyclo[2,2,1]heptadiene-2,5, which is the initial reagent in the synthesis of tetramethoxyethylene, and is a powerful reducing agent and methylating agent. The method involves re-etherification of 7-tetrabutoxynorbornanediene (7-t-BuO-NBD) by methanol in the presence tetrachloromethane and Mo-containing catalyst Mo(CO)6, with subsequent oxidation of intermediate 7-methoxynorbornanediene by methylhypochlorite, formed in situ from tetrachloromethane and methanol. The reaction is carried out at 80-100°C for 2 hours and molar ratio [Mo(CO)6]:[t-BuO-NBD]:[CCl4]:[MeOH]=1:100:100÷200:100÷400.
EFFECT: method allows shortening the duration of the reaction, consumption of toxic reagents, simplification and reduction of expenses on the stage of separating the target product.
1 tbl, 1 ex
Title | Year | Author | Number |
---|---|---|---|
METHOD FOR PREPARING CYCLOHEPTATRIENE-1,3,5 | 2005 |
|
RU2285689C1 |
4-VINYLCYCLOHEXENE-1 SYNTHESIS METHOD | 2008 |
|
RU2378243C1 |
5-ACETYLPYRROLE-2-CARBOXYLIC ACID METHYL ETHER SYNTHESIS METHOD | 2008 |
|
RU2404162C2 |
PRODUCTION METHOD FOR METHYL ETHERS OF 2-THIOPHEN CARBONIC ACID AND ITS DERIVATIVES | 2007 |
|
RU2359968C2 |
METHOD OF PRODUCING DIMETHYL ETHER OF 2,5-THIOPHENE DICARBOXYLIC ACID FROM 2-THIOPHENE CARBOXYLIC ACID | 2008 |
|
RU2402541C2 |
PROCESS FOR PREPARING 1-CHLOROADAMANTANE | 1996 |
|
RU2126784C1 |
METHOD FOR PREPARING 3-DICHLOROMETHYLPYRIDINE | 2006 |
|
RU2316547C1 |
METHOD FOR PREPARING ACETOPHENONE (METHYLPHENYL KETONE) | 2002 |
|
RU2237055C2 |
1-DICHLOROMETHYLISOQUINOLINE SYNTHESIS METHOD | 2008 |
|
RU2402535C2 |
METHOD OF PRODUCING ADAMANTANOL-1 | 2010 |
|
RU2448942C2 |
Authors
Dates
2008-08-20—Published
2006-06-01—Filed