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18162-48-6872-50-4Methylene ChloridenaphthaleneTHFTitanium Dioxide
ChemicalBook CAS DataBase List BIS THF Nitro Derivative 1
288296-64-0

BIS THF Nitro Derivative 1 synthesis

8synthesis methods
5070-13-3 Synthesis
BIS(4-NITROPHENYL) CARBONATE

5070-13-3
255 suppliers
$5.00/5g

156928-09-5 Synthesis
(3R,3aS,6aR)-hexahydrofuro[2,3-b]furan-3-ol

156928-09-5
149 suppliers
$80.00/1g

BIS THF Nitro Derivative 1

288296-64-0
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Yield:288296-64-0 160 g

Reaction Conditions:

with triethylamine in dichloromethane at 20 - 30;

Steps:

11 Preparation of (3R,3aS,6aR)-Hexahydrofuro[2,3-b]-furan-3-yl-4-nitrophenyl carbonate (2)

Example 11
Preparation of (3R,3aS,6aR)-Hexahydrofuro[2,3-b]-furan-3-yl-4-nitrophenyl carbonate (2)
To the solution of (3R,3aS,6aR)-Hexahydrofuro[2,3-b]furan-3-ol (1,100 g) and Bis-nitrophenyl carbonate (257.2 g) in methylene dichloride (1200 mL), triethylamine solution (132 g in 300 mL of methylene dichloride) was added slowly at 20-30° C. for 2-3hours.
Maintained the reaction at the same temperature for 8-10 hours, after completion of reaction water (500 mL) was added for 30-60 minutes and settled the reaction mass then separated the organic layer.
Organic layer was washed with 10% acetic acid (100 mL) and 10% sodium chloride solution (500 mL), distilled the organic layer and co distilled with ethyl acetate (100mL).
Ethyl acetate (300 mL) was added to the distillate and heated to 50-55° C. for 30-45 minutes to get clear solution, the solution was cooled to 5-10° C. and maintained at the same temperature for 60 minutes.
The obtained solid was filtered, washed with ethanol (100 mL) and dried the wet material at 40-45° C. for 10-14 hours to get title compound 2 (yield 160 g).

References:

US2014/350270,2014,A1 Location in patent:Paragraph 0059

7693-46-1 Synthesis
4-Nitrophenyl chloroformate

7693-46-1
430 suppliers
$18.00/5g

(3S,3aR,6aS)-Hexahydrofuro[2,3-b]furan-3-ol

156928-10-8
15 suppliers
$180.00/10mg

BIS THF Nitro Derivative 1

288296-64-0
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References
ethyl 2-(4,5-dihydrofuran-3-yl)-2-oxoacetate

96406-00-7
1 suppliers
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BIS THF Nitro Derivative 1

288296-64-0
16 suppliers
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References
3-Furanacetic acid, 3-bromo-2-ethoxytetrahydro-α-oxo-, ethyl ester

1378929-89-5
0 suppliers
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BIS THF Nitro Derivative 1

288296-64-0
16 suppliers
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References
109789-19-7 Synthesis
2,3,3a,4,5,6a-hexahydrofuro[2,3-b]furan-4-ol

109789-19-7
12 suppliers
inquiry

BIS THF Nitro Derivative 1

288296-64-0
16 suppliers
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References

BIS THF Nitro Derivative 1 Related Search:

[(3R,3aS,6aR)-Hydroxyhexahydrofuro[2,3-β]furanyl Succinimidyl Carbonate Darunavir ethanolate FURO[3,4-B]FURAN-2(3H)-ONE, TETRAHYDRO-4-METHOXY-, (3AS,4S,6AR)-