3b,5-二羟基-6b,7b:15b,16b-二亚甲基-5b-雄甾烷-17-酮

3b,5-二羟基-6b,7b:15b,16b-二亚甲基-5b-雄甾烷-17-酮性质、用途与生产工艺

生产方法 

82543-15-5

74-95-3

82543-16-6

在氮气保护下，将锌粉（135.00g，2.065mol）和溴化铜（I）（5.00g，0.035mol）悬浮于1,2-二甲氧基乙烷（1820mL）中。将混合物加热至75℃并搅拌20分钟。随后加入(3b,5b,15a,16a)-15,16-二氢-3,5-二羟基-3'H-环丙并[15,16]雄甾-6,15-二烯-17-酮（100.00g，0.316mol），继续搅拌15分钟。接着，向体系中加入乙酸（4.5mL，0.078mol）和异丙醇（9.5mL，0.124mol），并在72℃下搅拌。缓慢滴加二溴甲烷（334g，1.921mol）在1,2-二甲氧基乙烷（114mL）中的溶液，控制滴加速度以维持反应温度在约75℃。搅拌反应混合物1小时，直至TLC分析显示原料完全转化。加入乙酸乙酯（2500mL）后，将体系冷却至0-5℃。缓慢加入5%乙酸水溶液（2500mL），继续搅拌30分钟。过滤收集固体，分离液相。水层用乙酸乙酯（1250mL，500mL）各萃取两次，合并有机相后用蒸馏水（2×2500mL）洗涤两次并分离。在45℃减压下除去有机溶剂，残余物溶于二异丙醚（560mL）中，搅拌后过滤，并用二异丙醚洗涤两次。将所得(2S,4aR,4bS,6aS,7aS,8aS,8bS,8cR,8dR,9aR,9bR)-2.9b-二羟基-4a,6a-二甲基十八烷基-7H-环丙烷[4,5]环戊[1,2-a]环丙烷[l]菲蒽7-酮在45℃下真空干燥，得到产物74.50g（0.225mol，收率71%）。产物经1H-NMR和13C-NMR确认结构，HPLC-MS（ESI）分析显示[M + Na]+ = 353和[2M + Na]+ = 683。

参考文献：

[1] Patent: EP2019114, 2009, A1. Location in patent: Page/Page column 11

[2] Patent: US2005/192450, 2005, A1. Location in patent: Page/Page column 6-7

[3] Patent: EP1571153, 2005, A2. Location in patent: Page/Page column 4; 9; 14

3b,5-二羟基-6b,7b:15b,16b-二亚甲基-5b-雄甾烷-17-酮 上下游产品信息

上游原料

下游产品

3b,5-二羟基-6b,7b:15b,16b-二亚甲基-5b-雄甾烷-17-酮 生产厂家

82543-16-6, 3b,5-二羟基-6b,7b:15b,16b-二亚甲基-5b-雄甾烷-17-酮 相关搜索:

• Steroids
• Pharmaceuticals
• Intermediates & Fine Chemicals
• 杂质对照品
• 抑制剂
• 医用原料
• 医药原料
• 屈螺酮中间体Q5 82543-16-6
• 3β,5-dihydroxy-6β,7β;15β,16β-dimethylene-5β-androstan-17-one
• Q5(Drospirenone)
• 屈螺酮Q5
• 屈螺酮杂质N2
• 化合物 (2S,4AR,4BS,6AS,7AS,8AS,8BS,8CR,8DR,9AR,9BR)-2,9B-DIHYDROXY-4A,6A-DIMETHYLHEXADECAHYDRO-1H-CYCLOPROPA[4,5]CYCLOPENTA[1,2-A]CYCLOPROPA[L]PHENANTHREN-7(7AH)-ONE
• 3B,5-二羟基-6B,7B:15B,16B-二亚甲基-5B-雄甾烷-17-酮(屈螺酮中间体Q5)
• 6Β,7Β,15Β,16Β-二亚甲基-3Β,5Β-二羟基雄烷-17-酮
• 双环物
• Q5/D8
• 屈螺酮中间体D8/Q5
• (2S,4AR,4BS,6AS,7AS,8AS,8BS,8CR,8DR,9AR,9BR)-2.9B-二羟基-4A,6A-二甲基十八烷基-7H-环丙烷[4,5]环戊[1,2-A]环丙烷[L]菲蒽7-酮
• DROSPIRENONE IMPURITY 5
• 3b,5-二羟基-6b,7b:15b,16b-二亚甲基-5b-雄甾烷-17-酮
• 3Β,5-二羟基-6Β,7Β:15Β,16Β-二亚甲基-5Β-雄甾烷-17-酮
• 屈螺酮中间体Q5
• 82543-16-6
• 3β,5-dihydroxy-6β,7β
• 3β,5β-Dihydroxy-6β,7β
• (1R,5R,7S,10R,14S,16S,18S)-5,7-dihydroxy-10,14-dimethylhexacyclo[9.8.0.02,?.0?,1?.01?,1?.01?,1?]nonadecan-15-one
• Drospirosterone impurity 15
• Drospirenone Impurity N2
• 15beta,16beta-dimethylene-5beta-androst-17-one
• 3b,5-Dihydroxy-6b,7b:15b,16b-dimethylene-5b- androstan-17-one(Drospirenone Int.Q5)
• 15β,16β-dimethylene-5β-androstan- 17-one (Q5)
• 15β,?16β-?dimethylene-?5β-?androst-?17-?one
• 3b,5- dihydroxy -6b,7b:15b,16b- dimethyl -5b- androstane -17- one
• 5-Dihydroxy-6b,7b:15b,16b-dimethylene-5b-androstan-17-one
• (1R,2R,4R,5R,7S,10R,11S,14S,16S,18S,19S)-5,7-Dihydroxy-10,14-dimethylhexacyclo[9.8.0.02,4.05,10.014,19.016,18]nonadecan-15-one
• D8/Q5
• 3b,5-Dihydroxy-6b,7b:15b,16b-dimethylene-5b-androstan-17-one 82543-16-6
• 3b,5-Dihydroxy-6b,7b
• 15b,16b-dimethylene-5b-androstan-17-one
• 3B,5-DIHYDROXY-6B,7B:15B,16B-DIMETHYLENE-5B-ANDROSTAN-17-ONE CAS 82543-16-6
• 6β,7β,15β,16β-Dimethylene-3β,5β-dihydroxyandrostan-17-one
• 17H-Dicyclopropa[6,7:15,16]cyclopenta[a]phenanthren-17-one, octadecahydro-3,5-dihydroxy-10,13-dimethyl-, (3S,5R,6R,7R,8R,9S,10R,13S,14S,15S,16S)-
• Drospirenone Impurity 5
• Drospirenone intermediate Q5
• D8/Q5:15β,16β-dimethylene-5β-androstan-17-one (Drospirenone Intermediate)
• 15beta,16beta-dimethylene-androst-17-one
• (2S,4aR,4bS,6aS,7aS,8aS,8bS,8cR,8dR,9aR,9bR)-2,9b-Dihydroxy-4a,6a-diMethylhexadecahydro-1H-cyclopropa[4,5]cyclopenta[1,2-a]cyclopropa[l]phenanthren-7(7aH)-one
• 3B,5-DIHYDROXY-6B,7B,15B,16B-DIMETHYLENE-5B-ANDROST-17-ONE
• [3S-(3α,5α,6β,7β,8α,9β,10α,13α,14β,15β,16β)]-octadecahydro-3,5-dihydroxy-10,13-diMethyl-17H-dicyclopropa[6,7:15,16]cyclopenta[a]phenanthren-17-one
• 15β,16β-diMethylene-5β-androstan-17-one(Q5)
• 15β,16β-dimethylene-5β-androst -17-one
• 15β, 16β-methylene-androst-17-one
• 3β,5-dihydroxy-6β,7β
• 15β,16β-dimethylene-5β-androstan-17-one
• 7bydroxy-15b,16b-methylene-3b-pivaloyloxy-5 androsten-17-one
• 6,7,15,16 dimethylen 3,5, dihydroxy androstan 17 dion
• 6,7,15,16-Dimethylene-3,5-dihydroxyandrostan-17-one