5,6-Dimethoxy-2-nitroso-2,3-dihydro-1H-inden-1-one synthesis
- Product Name:5,6-Dimethoxy-2-nitroso-2,3-dihydro-1H-inden-1-one
- CAS Number:2107-85-9
- Molecular formula:C11H11NO4
- Molecular Weight:221.21
2107-69-9
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Yield:2107-85-9 95.4%
Reaction Conditions:
with hydrogenchloride;isopentyl nitrite in methanol;lithium hydroxide monohydrate at 45 - 50; for 10 h;Large scale;Temperature;
Steps:
1-3 Synthesis Compound 2
Methanol 772kg (10V) was added to the 2000L reactor,Add 75.0Kg compound 1 (1.0eq) under stirring, stir to dissolve,Then isoamyl nitrite 91.4Kg (2.0eq),The temperature was raised to 50°C with stirring, and then 11.7Kg (0.3eq) of hydrochloric acid was slowly added dropwise.The temperature was controlled at 45 °C, and the reaction was stirred for 10 h.Then it was cooled to 20°C, kept stirring for 2h, filtered, washed with methanol,The filter cake was dried at 45°C to obtain compound 2 in a yield of 95.4%,HPLC: 94.74%
References:
CN114591238,2022,A Location in patent:Paragraph 0073-0076; 0090-0092; 0099-0101
2107-70-2
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