(5Z)-1-羟基-3-(2-甲基丙基)-5-(2-甲基丙亚基)吡嗪-2,6-二酮合成路线 （共 11 条）
反应条件
trifluoroacetic acid in dichloromethane
参考文献
Singh, Sheo B.
Tetrahedron Letters, 1995 , vol. 36, # 12 p. 2009 - 2012
反应条件
1.1: DIPEA / acetonitrile / 20 - 60 °C
2.1: 101.5 g / DIPEA / acetonitrile / 24 h / 70 °C
3.1: 93.7 percent / TFA / CH2Cl2 / 70 h / 20 °C
4.1: TEA; DCC / CH2Cl2 / 20 h / 20 °C
5.1: hydroxylamine / ethanol; tetrahydrofuran / 3 h / 20 °C / pH 6.0
6.1: ethanol; H2O / Heating
7.1: 54 g / DIPEA / CH2Cl2 / 2 h / -40 °C
8.1: LHMDS / tetrahydrofuran; hexamethylphosphoric acid triamide / 3 h / -78 °C
8.2: 63.3 percent / 2 h
9.1: 4.5 g / DIPEA; DMAP / CH2Cl2 / -23 - 20 °C
10.1: 1.53 g / DBU / toluene / 0 - 50 °C
11.1: 30 percent / DDQ / CH2Cl2; H2O / 20 °C
12.1: 2 mg / TFA / CH2Cl2 / 0 - 20 °C
View Scheme
参考文献
Singh; Tomassini
Journal of Organic Chemistry, 2001 , vol. 66, # 16 p. 5504 - 5516
反应条件
1.1: 101.5 g / DIPEA / acetonitrile / 24 h / 70 °C
2.1: 93.7 percent / TFA / CH2Cl2 / 70 h / 20 °C
3.1: TEA; DCC / CH2Cl2 / 20 h / 20 °C
4.1: hydroxylamine / ethanol; tetrahydrofuran / 3 h / 20 °C / pH 6.0
5.1: ethanol; H2O / Heating
6.1: 54 g / DIPEA / CH2Cl2 / 2 h / -40 °C
7.1: LHMDS / tetrahydrofuran; hexamethylphosphoric acid triamide / 3 h / -78 °C
7.2: 63.3 percent / 2 h
8.1: 4.5 g / DIPEA; DMAP / CH2Cl2 / -23 - 20 °C
9.1: 1.53 g / DBU / toluene / 0 - 50 °C
10.1: 30 percent / DDQ / CH2Cl2; H2O / 20 °C
11.1: 2 mg / TFA / CH2Cl2 / 0 - 20 °C
View Scheme
参考文献
Singh; Tomassini
Journal of Organic Chemistry, 2001 , vol. 66, # 16 p. 5504 - 5516
反应条件
1.1: 54 g / DIPEA / CH2Cl2 / 2 h / -40 °C
2.1: LHMDS / tetrahydrofuran; hexamethylphosphoric acid triamide / 3 h / -78 °C
2.2: 63.3 percent / 2 h
3.1: 4.5 g / DIPEA; DMAP / CH2Cl2 / -23 - 20 °C
4.1: 1.53 g / DBU / toluene / 0 - 50 °C
5.1: 30 percent / DDQ / CH2Cl2; H2O / 20 °C
6.1: 2 mg / TFA / CH2Cl2 / 0 - 20 °C
View Scheme
参考文献
Singh; Tomassini
Journal of Organic Chemistry, 2001 , vol. 66, # 16 p. 5504 - 5516
反应条件
1.1: TEA; DCC / CH2Cl2 / 20 h / 20 °C
2.1: hydroxylamine / ethanol; tetrahydrofuran / 3 h / 20 °C / pH 6.0
3.1: ethanol; H2O / Heating
4.1: 54 g / DIPEA / CH2Cl2 / 2 h / -40 °C
5.1: LHMDS / tetrahydrofuran; hexamethylphosphoric acid triamide / 3 h / -78 °C
5.2: 63.3 percent / 2 h
6.1: 4.5 g / DIPEA; DMAP / CH2Cl2 / -23 - 20 °C
7.1: 1.53 g / DBU / toluene / 0 - 50 °C
8.1: 30 percent / DDQ / CH2Cl2; H2O / 20 °C
9.1: 2 mg / TFA / CH2Cl2 / 0 - 20 °C
View Scheme
参考文献
Singh; Tomassini
Journal of Organic Chemistry, 2001 , vol. 66, # 16 p. 5504 - 5516
反应条件
1.1: ethanol; H2O / Heating
2.1: 54 g / DIPEA / CH2Cl2 / 2 h / -40 °C
3.1: LHMDS / tetrahydrofuran; hexamethylphosphoric acid triamide / 3 h / -78 °C
3.2: 63.3 percent / 2 h
4.1: 4.5 g / DIPEA; DMAP / CH2Cl2 / -23 - 20 °C
5.1: 1.53 g / DBU / toluene / 0 - 50 °C
6.1: 30 percent / DDQ / CH2Cl2; H2O / 20 °C
7.1: 2 mg / TFA / CH2Cl2 / 0 - 20 °C
View Scheme
参考文献
Singh; Tomassini
Journal of Organic Chemistry, 2001 , vol. 66, # 16 p. 5504 - 5516
反应条件
1.1: LHMDS / tetrahydrofuran; hexamethylphosphoric acid triamide / 3 h / -78 °C
1.2: 63.3 percent / 2 h
2.1: 4.5 g / DIPEA; DMAP / CH2Cl2 / -23 - 20 °C
3.1: 1.53 g / DBU / toluene / 0 - 50 °C
4.1: 30 percent / DDQ / CH2Cl2; H2O / 20 °C
5.1: 2 mg / TFA / CH2Cl2 / 0 - 20 °C
View Scheme
参考文献
Singh; Tomassini
Journal of Organic Chemistry, 2001 , vol. 66, # 16 p. 5504 - 5516
反应条件
1.1: 93.7 percent / TFA / CH2Cl2 / 70 h / 20 °C
2.1: TEA; DCC / CH2Cl2 / 20 h / 20 °C
3.1: hydroxylamine / ethanol; tetrahydrofuran / 3 h / 20 °C / pH 6.0
4.1: ethanol; H2O / Heating
5.1: 54 g / DIPEA / CH2Cl2 / 2 h / -40 °C
6.1: LHMDS / tetrahydrofuran; hexamethylphosphoric acid triamide / 3 h / -78 °C
6.2: 63.3 percent / 2 h
7.1: 4.5 g / DIPEA; DMAP / CH2Cl2 / -23 - 20 °C
8.1: 1.53 g / DBU / toluene / 0 - 50 °C
9.1: 30 percent / DDQ / CH2Cl2; H2O / 20 °C
10.1: 2 mg / TFA / CH2Cl2 / 0 - 20 °C
View Scheme
参考文献
Singh; Tomassini
Journal of Organic Chemistry, 2001 , vol. 66, # 16 p. 5504 - 5516
反应条件
1.1: hydroxylamine / ethanol; tetrahydrofuran / 3 h / 20 °C / pH 6.0
2.1: ethanol; H2O / Heating
3.1: 54 g / DIPEA / CH2Cl2 / 2 h / -40 °C
4.1: LHMDS / tetrahydrofuran; hexamethylphosphoric acid triamide / 3 h / -78 °C
4.2: 63.3 percent / 2 h
5.1: 4.5 g / DIPEA; DMAP / CH2Cl2 / -23 - 20 °C
6.1: 1.53 g / DBU / toluene / 0 - 50 °C
7.1: 30 percent / DDQ / CH2Cl2; H2O / 20 °C
8.1: 2 mg / TFA / CH2Cl2 / 0 - 20 °C
View Scheme
参考文献
Singh; Tomassini
Journal of Organic Chemistry, 2001 , vol. 66, # 16 p. 5504 - 5516
反应条件
1: 1.53 g / DBU / toluene / 0 - 50 °C
2: 30 percent / DDQ / CH2Cl2; H2O / 20 °C
3: 2 mg / TFA / CH2Cl2 / 0 - 20 °C
View Scheme
参考文献
Singh; Tomassini
Journal of Organic Chemistry, 2001 , vol. 66, # 16 p. 5504 - 5516
