Technology Process of 9-(4-methylphenyl)thiocarboxylacyl-4-dedimethylamino-minocycline
There total 6 articles about 9-(4-methylphenyl)thiocarboxylacyl-4-dedimethylamino-minocycline which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
C26H25N3O10; sodium p-thiocresolate;
In
1-methyl-pyrrolidin-2-one;
at 20 - 80 ℃;
for 3.5h;
With
hydrogenchloride;
In
water;
pH=1;
- Guidance literature:
-
Multi-step reaction with 6 steps
1.1: sodium hydrogencarbonate / water / pH 6.5 - 7
2.1: methyl iodide / tetrahydrofuran / 16 h / 40 - 45 °C / Inert atmosphere
3.1: trifluoroacetic acid; zinc / water; N,N-dimethyl-formamide / 3 h / 5 °C
3.2: pH 3.5
4.1: methanesulfonic acid; iodine; silver sulfate / 3 h / Inert atmosphere
4.2: pH 7
5.1: N-ethyl-N,N-diisopropylamine / tetrakis(triphenylphosphine) palladium(0) / 1-methyl-pyrrolidin-2-one / 60 °C / 20 - 760.05 Torr / Inert atmosphere
6.1: 1-methyl-pyrrolidin-2-one / 3.5 h / 20 - 80 °C
6.2: pH 1
With
methanesulfonic acid; iodine; sodium hydrogencarbonate; silver sulfate; N-ethyl-N,N-diisopropylamine; trifluoroacetic acid; zinc; methyl iodide;
tetrakis(triphenylphosphine) palladium(0);
In
tetrahydrofuran; 1-methyl-pyrrolidin-2-one; water; N,N-dimethyl-formamide;
- Guidance literature:
-
Multi-step reaction with 3 steps
1.1: methanesulfonic acid; iodine; silver sulfate / 3 h / Inert atmosphere
1.2: pH 7
2.1: N-ethyl-N,N-diisopropylamine / tetrakis(triphenylphosphine) palladium(0) / 1-methyl-pyrrolidin-2-one / 60 °C / 20 - 760.05 Torr / Inert atmosphere
3.1: 1-methyl-pyrrolidin-2-one / 3.5 h / 20 - 80 °C
3.2: pH 1
With
methanesulfonic acid; iodine; silver sulfate; N-ethyl-N,N-diisopropylamine;
tetrakis(triphenylphosphine) palladium(0);
In
1-methyl-pyrrolidin-2-one;