Technology Process of 9,9',9'',9'''-tetrabenzyl-6'''-chloro-[6,8',6',8'',6''.8''']quaterpurine
There total 10 articles about 9,9',9'',9'''-tetrabenzyl-6'''-chloro-[6,8',6',8'',6''.8''']quaterpurine which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
9-benzyl-6-chloro-8-iodo-9H-purine;
With
isopropylmagnesium chloride lithium chloride complex;
In
tetrahydrofuran;
at -40 ℃;
for 0.25h;
With
zinc dibromide;
In
tetrahydrofuran;
at -40 - 20 ℃;
9,9',9''-tribenzyl-6''-iodo-[6,8',6',8'']terpurine;
With
tris(dibenzylideneacetone)dipalladium (0);
In
tetrahydrofuran;
at 45 ℃;
for 16h;
DOI:10.1002/ejoc.200600724
- Guidance literature:
-
Multi-step reaction with 7 steps
1.1: 28.0 g / TMSCl; tert-butyl nitrite; benzyltriethylammonium chloride / CH2Cl2 / 27 h / 20 °C
2.1: 88 percent / aq. HI / 1 h / 0 °C
3.1: 1,2-dibromoethane; TMSCl; zinc / N,N-dimethyl-acetamide / 0.04 h / 20 °C
3.2: 61 percent / Pd2(dba)3; tfp / tetrahydrofuran; N,N-dimethyl-acetamide / 16 h / 45 °C
4.1: 100 percent / aq. HI / 1 h / 0 °C
5.1: iPrMgBr*LiCl / tetrahydrofuran / 0.25 h / -40 °C
5.2: ZnBr2 / tetrahydrofuran / -40 - 20 °C
5.3: 77 percent / Pd2(dba)3 / tetrahydrofuran / 16 h / 45 °C
6.1: 95 percent / aq. HI / 1 h / 0 °C
7.1: iPrMgBr*LiCl / tetrahydrofuran / 0.25 h / -40 °C
7.2: ZnBr2 / tetrahydrofuran / -40 - 20 °C
7.3: 46 percent / Pd2(dba)3 / tetrahydrofuran / 16 h / 45 °C
With
chloro-trimethyl-silane; tert.-butylnitrite; isopropylmagnesium chloride lithium chloride complex; N-benzyl-N,N,N-triethylammonium chloride; hydrogen iodide; ethylene dibromide; zinc;
In
tetrahydrofuran; dichloromethane; N,N-dimethyl acetamide;
5.1: Negishi cross-coupling reaction / 7.1: Negishi cross-coupling reaction;
DOI:10.1002/ejoc.200600724
- Guidance literature:
-
Multi-step reaction with 6 steps
1.1: 88 percent / aq. HI / 1 h / 0 °C
2.1: 1,2-dibromoethane; TMSCl; zinc / N,N-dimethyl-acetamide / 0.04 h / 20 °C
2.2: 61 percent / Pd2(dba)3; tfp / tetrahydrofuran; N,N-dimethyl-acetamide / 16 h / 45 °C
3.1: 100 percent / aq. HI / 1 h / 0 °C
4.1: iPrMgBr*LiCl / tetrahydrofuran / 0.25 h / -40 °C
4.2: ZnBr2 / tetrahydrofuran / -40 - 20 °C
4.3: 77 percent / Pd2(dba)3 / tetrahydrofuran / 16 h / 45 °C
5.1: 95 percent / aq. HI / 1 h / 0 °C
6.1: iPrMgBr*LiCl / tetrahydrofuran / 0.25 h / -40 °C
6.2: ZnBr2 / tetrahydrofuran / -40 - 20 °C
6.3: 46 percent / Pd2(dba)3 / tetrahydrofuran / 16 h / 45 °C
With
chloro-trimethyl-silane; isopropylmagnesium chloride lithium chloride complex; hydrogen iodide; ethylene dibromide; zinc;
In
tetrahydrofuran; N,N-dimethyl acetamide;
4.1: Negishi cross-coupling reaction / 6.1: Negishi cross-coupling reaction;
DOI:10.1002/ejoc.200600724