1,4-dioxa-10-azadispiro[4.2.4.2]tetradecan-11-one synthesis
- Product Name:1,4-dioxa-10-azadispiro[4.2.4.2]tetradecan-11-one
- CAS Number:914780-95-3
- Molecular formula:C11H17NO3
- Molecular Weight:211.26
![Ethyl 2-(8-(nitromethyl)-1,4-dioxaspiro[4.5]decan-8-yl)acetate](/CAS/20180703/GIF/1246508-12-2.gif)
1246508-12-2
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Yield:914780-95-3 100%
Reaction Conditions:
with hydrogen;triethylamine in methanol at 20;
Steps:
27.3 Step 3: Synthesis of 1,4-dioxa-10-azadispiro[4.2.48.25]tetradecan-11-one:
Into a 500-mL round-bottom flask, was placed ethyl 2-[8-(nitromethyl)-l,4- dioxaspiro[4.5]decan-8-yl]acetate (5 g, 17.40 mmol, 1 equiv), methanol (200 mL), Raney-Ni (1 g), TEA (5 g, 49.41 mmol, 2.84 equiv), hydrogen (500 mL). The resulting solution was stirred overnight at RT. The solids were filtered out. The resulting mixture was concentrated under vacuum. This resulted in 4 g (100%) of the title compound as a white solid. Analytical Data: NMR (300 MHz, Chloroform-i ) δ 6.35 (s, 1H), 3.96 (s, 4H), 3.21 (s, 2H), 2.23 (s, 2H), 1.79 - 1.60 (m, 8H).
References:
WO2017/181177,2017,A1 Location in patent:Paragraph 0568; 0575-0576
![Methyl 2-(8-(nitroMethyl)-1,4-dioxaspiro[4.5]decan-8-yl)acetate](/CAS/20150408/GIF/914780-94-2.gif)
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![1,4-Dioxaspiro[4.5]decan-8-one](/CAS/GIF/4746-97-8.gif)
4746-97-8
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$5.00/1g
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![ethyl 2-(1,4-dioxaspiro[4.5]decan-8-ylidene)acetate](/CAS/GIF/51656-91-8.gif)
51656-91-8
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$37.00/100mg
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![Methyl 2-(1,4-dioxaspiro[4.5]decan-8-ylidene)acetate](/CAS/20150408/GIF/172270-85-8.gif)
172270-85-8
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