Technology Process of 1,3-Dioxaspiro[4.5]decan-7-one,2,2,6,6,8-pentamethyl-,(5S)-(9CI)
There total 10 articles about 1,3-Dioxaspiro[4.5]decan-7-one,2,2,6,6,8-pentamethyl-,(5S)-(9CI) which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
Multi-step reaction with 3 steps
1.1: tBuLi / tetrahydrofuran / 0.08 h / -78 °C
1.2: H2O2; KHCO3; KF / tetrahydrofuran; methanol / 10 h / 20 °C
2.1: CSA / 1 h / 20 °C
2.2: Dess-Martin periodinane / CH2Cl2 / 2 h / 20 °C
3.1: TMSOTf; DIPEA / CH2Cl2 / 2 h / -20 °C
3.2: MeLi / tetrahydrofuran / 0.5 h / 20 °C
3.3: tetrahydrofuran / 9 h / 0 - 20 °C
With
trimethylsilyl trifluoromethanesulfonate; camphor-10-sulfonic acid; tert.-butyl lithium; N-ethyl-N,N-diisopropylamine;
In
tetrahydrofuran; dichloromethane;
1.2: Tamao oxidation reaction / 2.2: Dess-Martin oxidation reaction;
DOI:10.1016/j.tetlet.2007.07.179
- Guidance literature:
-
(S)-2,2,6,6-Tetramethyl-1,3-dioxa-spiro[4.5]decan-7-one;
With
trimethylsilyl trifluoromethanesulfonate; N-ethyl-N,N-diisopropylamine;
In
dichloromethane;
at -20 ℃;
for 2h;
With
methyllithium;
In
tetrahydrofuran;
at 20 ℃;
for 0.5h;
methyl iodide;
In
tetrahydrofuran;
at 0 - 20 ℃;
for 9h;
Further stages.;
DOI:10.1016/j.tetlet.2007.07.179
- Guidance literature:
-
Multi-step reaction with 7 steps
1.1: 1H-imidazole / dichloromethane / Inert atmosphere
2.1: sodium iodide / acetone / Inert atmosphere; Reflux
3.1: tert.-butyl lithium / diethyl ether / -78 °C / Inert atmosphere
4.1: Inert atmosphere
4.2: Inert atmosphere; Acidic conditions
5.1: Inert atmosphere
6.1: triethylamine / Inert atmosphere
7.1: methyllithium / Inert atmosphere
With
1H-imidazole; methyllithium; tert.-butyl lithium; triethylamine; sodium iodide;
In
diethyl ether; dichloromethane; acetone;
4.1: |Tamao-Kumada Oxidation;
DOI:10.1002/chem.201404295
