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CAS No. : | 62965-35-9 | MDL No. : | MFCD00065574 |
Formula : | C11H21NO4 | Boiling Point : | - |
Linear Structure Formula : | C5H9O2NHCH(CO2H)C4H9 | InChI Key : | LRFZIPCTFBPFLX-SSDOTTSWSA-N |
M.W : | 231.29 | Pubchem ID : | 2734668 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
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* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
73% | With sodium hypochlorite; 2,2,6,6-Tetramethyl-1-piperidinyloxy free radical; Isopropyl acetate; sodium hydrogencarbonate; sodium bromide; at 0 - 25℃; | In a four-neck flask, 10.0 g (1.0 eq) of N-Boc-t-butyl ethylamine alcohol compound was added. Isopropyl acetate 100ml, sodium bromide 2.0eq, sodium bicarbonate 2.0eq, TMEPO 0.05eq, Cool to 0-5 C. Temperature control 0 ~ 5 C, sodium hypochlorite drops 1.2eq, about 1.0 ~ 1.5h drops, heat 2h, Warm up to 20 ~ 25 C, heat 1.0 ~ 2.0h. Sodium thiosulfate solid 0.6 eq was added and incubated for 0.5 h. The aqueous layer was further extracted with 20 ml isopropyl acetate and the phases separated. Add 20 ml of isopropyl acetate to the aqueous layer, add citric acid, adjust the pH to 2 to 3, separate the phases, extract the aqueous layer with 20 ml of x 2 isopropyl acetate, combine the organic layers, add 50 ml of water to wash, separate the phases, and then apply the organic layer. Dry with 0.5g anhydrous magnesium sulfate 0.5h, suction filtration, the filtrate was evaporated to dryness at 40 ~ 50 C, 40 ~ 50 C insulation, 5ml of isopropyl acetate was added, 25ml of heptane was added dropwise, slowly cooling and crystallization, 20 ~ 30 C heat 0.5h, suction filtration, washing, 7.8g boutique, yield 73%. Optical purity 100%. |
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