2,2,5-三甲基-1,3-二恶烷-5-甲酸合成路线 （共 12 条）
反应条件
1: 3-hydroxy-2-(hydroxymethyl)-2-methylpropionic acid With toluene-4-sulfonic acid in benzene Reflux; 2: 2,2-dimethoxy-propane in benzene 3 h;
参考文献
CADILA HEALTHCARE LIMITED
Patent: US2012/202988 A1, 2012 ;
Location in patent: Page/Page column 12 ;
反应条件
toluene-4-sulfonic acid
参考文献
Angewandte Chemie, International Edition, , vol. 48, p. 4047 - 4051
Angewandte Chemie, , vol. 121, p. 4107 - 4111
参考文献
American Home Products Corporation
Patent: US6277983 B1, 2001 ;
参考文献
Giri, Ramesh; Chen, Xiao; Yu, Jin-Quan
Angewandte Chemie - International Edition, 2005 , vol. 44, # 14 p. 2112 - 2115
反应条件
1: 80 percent / LiCl / PdCl2 / 16 h / Heating 2: H2SO4 / acetonitrile; H2O / 4 h / 20 °C 3: 78 percent / 1.5 h / 20 °C 4: 78 percent / Amano I Burkholderia cepacia lipase PC-D; molecular sieves 5 Angstroem / various solvent(s) / 48 h / 40 - 42 °C 5: 78 percent / MeOH / various solvent(s) View Scheme
参考文献
CADILA HEALTHCARE LIMITED; DAVE, Mayank, Ghanshyambhai; PANDEY, Bipin
Patent: WO2011/51960 A2, 2011 ;
反应条件
1: 1.) 1,1-carbonylimidazole / 1.) CH2Cl2, 10 min, 2.) room temperature, 20 h 2: 86 percent / tetrahydrofuran / 0.5 h / Ambient temperature View Scheme
参考文献
Journal of Organic Chemistry, , vol. 57, # 9 p. 2566 - 2574
→
162635-03-2(1R,2R,4S)-4-{(2R)-2-[(1R,9S,12S,15R,16E,18R,19R,21R,23S,24E,26E,28E,30S,32S,35R)-1,18-二羟基-19,30-二甲氧基-15,17,21,23,29,35-六甲基-2,3,10,14,20-五氧代-11,36-二氧杂-4-氮杂三环[30.3.1.04,9]三十六碳-16,24,26,28-四烯-12-基]丙基}-2-甲氧基环己基2,2,5-三甲基-1,3-二恶烷-5-羧酸酯
反应条件
1: 2,2-bis(hydroxymethyl)propionic acid isopropylidene ketal With 2,4,6-trichlorobenzoyl chloride; triethylamine in tetrahydrofuran T=0 - 20°C; 5 h; 2: [14C]-Rapamycin With 4-(N,N-dimethlyamino)pyridine in benzene T=20°C;
参考文献
Wyeth
Patent: EP1266899 A2, 2002 ;
Location in patent: Example 10 ;
→
162635-03-2(1R,2R,4S)-4-{(2R)-2-[(1R,9S,12S,15R,16E,18R,19R,21R,23S,24E,26E,28E,30S,32S,35R)-1,18-二羟基-19,30-二甲氧基-15,17,21,23,29,35-六甲基-2,3,10,14,20-五氧代-11,36-二氧杂-4-氮杂三环[30.3.1.04,9]三十六碳-16,24,26,28-四烯-12-基]丙基}-2-甲氧基环己基2,2,5-三甲基-1,3-二恶烷-5-羧酸酯
反应条件
1: 80 percent / LiCl / PdCl2 / 16 h / Heating 2: Amano II Burkholderia cepacia lipase PS-C; molecular sieves 5 Angstroem / various solvent(s) / 48 h / 42 - 43 °C View Scheme
参考文献
Gu, Jianxin; Ruppen, Mark E.; Cai, Ping
Organic Letters, 2005 , vol. 7, # 18 p. 3945 - 3948
反应条件
vinyl acetate; lithium chloride; palladium dichloride in methanol
16 h; Heating / reflux;
参考文献
Wyeth
Patent: US2005/234086 A1, 2005 ;
Location in patent: Page/Page column 13 ;
反应条件
lithium chloride; palladium dichloride
16 h; Heating;
参考文献
Gu, Jianxin; Ruppen, Mark E.; Cai, Ping
Organic Letters, 2005 , vol. 7, # 18 p. 3945 - 3948
