Cyclosporin A-Derivative 1 Free base synthesis
- Product Name:Cyclosporin A-Derivative 1 Free base
- CAS Number:286852-20-8
- Molecular formula:C65H117N11O14
- Molecular Weight:1276.69
83602-41-9
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Yield:286852-20-8 170 g
Reaction Conditions:
with trimethoxonium tetrafluoroborate in dichloromethane at 0 - 20; for 20 h;
Steps:
1.1b
Compound of formula (1-1) (250 g, 0.2 mole) was dissolved in anhydrous CH2Cl2 (2 L). Trimethyloxoniumtetrafluoroborate (89.12 g, 0.6 mol) was added at 0° C. and the reaction mixture was stirred at room temperature for 20 hrs. Methanol and water (1:1 mixture, 2.5 L) was added via a dropping funnel over 15 mins at 0° C. and then stirred at room temperature for 3 hrs. Reaction mixture was further diluted with 2 L of CH2Cl2 and 2 L of water. The organic layer was separated and washed with saturated Na2CO3 (2 L) and brine (2 L), and then dried over Na2SO4. The solvent was removed and the residue was purified on silica gel column to afford the compound of formula (1-2) (170 g, 92.5 HPLC purity). MS (ESI): 1276.8 m/z (M+1)
References:
US2016/51625,2016,A1 Location in patent:Paragraph 0392; 0393
67-56-1
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420-37-1
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59865-13-3
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