Technology Process of 33,35,37-trioxo-34,38-dimethoxy-4,26-dimethyl-36-<3-(methoxymethyl)phenyl>-1,7,11,19,23,29-hexaazaheptacyclo<27.3.1.12,6.17,11.113,17.119,23.124,28>octaconta-34(2),3,5,36(13),14,16,38(24),25,27-nonaene
There total 7 articles about 33,35,37-trioxo-34,38-dimethoxy-4,26-dimethyl-36-<3-(methoxymethyl)phenyl>-1,7,11,19,23,29-hexaazaheptacyclo<27.3.1.12,6.17,11.113,17.119,23.124,28>octaconta-34(2),3,5,36(13),14,16,38(24),25,27-nonaene which
guide to synthetic route it.
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synthetic route:
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84011-90-5
33,35,37-trioxo-34,38-dimethoxy-4,26-dimethyl-36-<3-(methoxymethyl)phenyl>-1,7,11,19,23,29-hexaazaheptacyclo<27.3.1.12,6.17,11.113,17.119,23.124,28>octaconta-34(2),3,5,36(13),14,16,38(24),25,27-nonaene
- Guidance literature:
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With
sodium hydride;
In
tetrahydrofuran;
at -78 - 25 ℃;
for 40h;
DOI:10.1021/ja00339a035
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84011-90-5
33,35,37-trioxo-34,38-dimethoxy-4,26-dimethyl-36-<3-(methoxymethyl)phenyl>-1,7,11,19,23,29-hexaazaheptacyclo<27.3.1.12,6.17,11.113,17.119,23.124,28>octaconta-34(2),3,5,36(13),14,16,38(24),25,27-nonaene
- Guidance literature:
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Multi-step reaction with 7 steps
1: 55 percent / ammonium sulfide 22percent / methanol / 0.67 h / Heating
2: 90 percent / pyridine / tetrahydrofuran / 30 h / Heating
3: 70 percent / NaOH, benzyltriethylammonium bromide / benzene; H2O / 96 h / 46 °C
4: 97.6 percent / iron powder, hydrochloric acid / ethanol; H2O / 3 h / Heating
5: CH2Cl2 / 48.5 h / slight initial warming
6: 61.8 percent / potassium tert-butoxide / 2-methyl-propan-2-ol / 15 h / 32 °C
7: 1.) sodium hydride / 1.) THF, reflux, 4 h; 2.) THF -78 deg C to rt, 40 h, 3.) MeOH, water, reflux
With
pyridine; hydrogenchloride; sodium hydroxide; ammonium sulfide; potassium tert-butylate; benzyltriethylammonium bromide; iron; sodium hydride;
In
tetrahydrofuran; methanol; ethanol; dichloromethane; water; tert-butyl alcohol; benzene;
DOI:10.1021/ja00329a059
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84011-90-5
33,35,37-trioxo-34,38-dimethoxy-4,26-dimethyl-36-<3-(methoxymethyl)phenyl>-1,7,11,19,23,29-hexaazaheptacyclo<27.3.1.12,6.17,11.113,17.119,23.124,28>octaconta-34(2),3,5,36(13),14,16,38(24),25,27-nonaene
- Guidance literature:
-
Multi-step reaction with 6 steps
1: 90 percent / pyridine / tetrahydrofuran / 30 h / Heating
2: 70 percent / NaOH, benzyltriethylammonium bromide / benzene; H2O / 96 h / 46 °C
3: 97.6 percent / iron powder, hydrochloric acid / ethanol; H2O / 3 h / Heating
4: CH2Cl2 / 48.5 h / slight initial warming
5: 61.8 percent / potassium tert-butoxide / 2-methyl-propan-2-ol / 15 h / 32 °C
6: 1.) sodium hydride / 1.) THF, reflux, 4 h; 2.) THF -78 deg C to rt, 40 h, 3.) MeOH, water, reflux
With
pyridine; hydrogenchloride; sodium hydroxide; potassium tert-butylate; benzyltriethylammonium bromide; iron; sodium hydride;
In
tetrahydrofuran; ethanol; dichloromethane; water; tert-butyl alcohol; benzene;
DOI:10.1021/ja00329a059