1-nitro-4-sulfooxy-benzene synthesis
- Product Name:1-nitro-4-sulfooxy-benzene
- CAS Number:1080-04-2
- Molecular formula:C6H5NO6S
- Molecular Weight:219.17
100-02-7
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Yield:1080-04-2 90%
Reaction Conditions:
with sulfur trioxide pyridine complex in tetrahydrofuran at 25; for 2 h;Reagent/catalyst;Temperature;Solvent;
Steps:
Example: Production of PNPS salt PNPS salts were synthesized under the conditions shown in TEST Nos. 1 to 7 in Table 1. [0043] Specifically, in the case of Test No. 3, the PNPS salt was synthesized in the following procedure. A 100 mL four-necked flask was substituted with Ar, and 50 mL of THF, 2.21 g (15.9 mmol; 318 mM) of p-nitrophenol, 3.13 g (19.7 mmol; 394 mM) of sulfur trioxide pyridine complex was added and the mixture was stirred at 25 ° C. for 2 hours (sulfation step). 1.78 g (15.9 mmol; 318 mM) of t-BuOK was further added and the mixture was stirred at 25 ° C. for 2 hours. Precipitation of crystals was observed (neutralization step). The resulting slurry was filtered and then crystallized with 10 mL of THF. The obtained wet crystals were dried under reduced pressure at 40 ° C. for 12 hours to obtain 4.32 g of dried crystals. After the sulfation step, a part of the reaction liquid was fractionated, When PNPS was quantified by HPLC, PNPS was found to be produced with a reaction yield of 90%. The purity of the PNPS salt was calculated by subjecting the obtained dried crystals to component analysis by HPLC. The isolation yield of PNPS-K was 77%.
References:
JP2017/119648,2017,A Location in patent:Paragraph 0043; 0046
330-13-2
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1080-04-2
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