ANTAL ARANYI,ZOLTN BNI,SNDOR MAH,CSABA SNTA,JNOS HORVTH,JNOS CSRGEI
申请号：
ARP140103652
公开号：
AR097878A1
申请日:
2014.10.01
申请国别(地区):
AR
年份:
2016
代理人:
摘要：
Claim formula compound (3). Characteristic 1: synthesis process of formula compound (1) (R means diethylamine or acetylene group) characteristic is (a) formula compound (2) (R means a group)dimethylamino or 2-methyl-1,3-dioxolan-2-yl) is reacted with 2-15 molar equivalents of methyl lithium in the presence of tetraalkylethylenediamine in a solvent of acetal ether or formaldehyde type or in a mixture thereof at a temperature between -78 - (-20) ºCthen the protected imine obtained as an intermediate is reacted with a strong mineral or organic acid at a temperature between 0 ° C and the boiling point of the organic solvent used, then the hydroxyl group at position 17 of the compound of formula (4) obtained (where the meaning of R is as described for formula (1)) is acetylated with acetic anhydride in a halogenated solvent, preferably dichloromethane, in the presence of 70% perchloric acid at a temperature between -78 - 0ºC, then the compound of formula ( 1) obtained (where the meaning of R is dimethylamino or acetyl group) in this case it is recrystallized from methanol or ethanol；or b) the hydroxyl group at position 5 of the compound of formula (2) (where the meaning of R is dimethylamino group or 2-methyl-1,3-dioxolan-2-yl) is silylated with chloromethylsilane in the presence of imidazole in a halogenated solvent, tetrahydrofuran or toluene, preferably in dichloromethane at room temperature； then the compound obtained from formula (3) (where the meaning of R is as described for formula (2)) is reacted with 2-15 molar equivalents of methyllithium in the presence of tetraalkylethylenediamine in a solvent of acetal ether type or formaldehyde or a mixture thereof at a temperature between -78 - (-20) ºC,then the protected imine obtained as an intermediate is reacted with a strong mineral or organic acid at a temperature between 0 ° C and the boiling point of the organic solvent used, then the hydroxyl group at position 17 of the compound of formula (4) obtained (where the
