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ChemicalBook CAS DataBase List 2H-Pyran, tetrahydro-4-(nitromethylene)-

2H-Pyran, tetrahydro-4-(nitromethylene)- synthesis

3synthesis methods
2H-Pyran-4-ol, tetrahydro-4-(nitromethyl)-

50289-14-0
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2H-Pyran, tetrahydro-4-(nitromethylene)-

105772-10-9
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Yield:105772-10-9 88.3%

Reaction Conditions:

with diethylamino-sulfur trifluoride in dichloromethane at 0; for 1 h;

Steps:

10 Preparation of Compound I-10:

Compound III-10 (20.0 g, 0.124 mol, 1.0 e.q.) was dissolved in 200 mL of DCM, and DAST (30.01 g, 0.186 mol, 1.5 e.q.) was added dropwise at 0 ° C, and the reaction was further stirred at 0 ° C for 1 h.The TLC test showed that the reaction of the starting material was complete. The reaction was quenched by the addition of saturated aqueous sodium carbonate. The organic phase was separated and dried over anhydrous sodium sulfate. The solvent was evaporated and evaporated to give the compound I-10 as a white solid 15.69 g. The yield was 88.3%.

References:

CN108863884,2018,A Location in patent:Paragraph 0096; 0097; 0100; 0101