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CAS No. : | 146256-98-6 | MDL No. : | MFCD06656201 |
Formula : | C12H19NO5 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | CWRFSVAKVCSOPI-UHFFFAOYSA-N |
M.W : | 257.28 | Pubchem ID : | 10868942 |
Synonyms : |
|
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: |
* 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 |
---|---|---|
85% | With sodium hydride In N,N-dimethyl-formamide at 0 - 5℃; for 2.66667 h; | 1000ml four-necked flask by adding Boc-pyrrolidone 120g, DMF 600ml, Stirring down to 0-5 , Sodium hydride was added to 26 g, 70.5 g of ethyl chloroformate was slowly added dropwise with stirring, 40min drop finished. 0-5 reaction 2h, TLC detection reaction is completed, Slowly add 3L ice water, With dilute hydrochloric acid to adjust the pH = 7 after ethyl acetate extraction, dry, Concentrated to give intermediate 1. Yield 85percent. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
10.8 g | With 2,6-di-tert-butyl-4-methyl-phenol In water; dimethyl sulfoxide; toluene for 6 h; | Ethyl N-Boc pyrrolidonecarboxylate (20.0 g) (compound of formula (II) wherein R is Et) was dissolved in toluene (30 ml) and dimethylsulfoxide Mixture and 20 mg of 3,5-di-tert-butyl-4-hydroxytoluene (BHT) was added.The resulting mixture was heated to 115 ° C (internal temperature) and water (4.2 ml, 3.0 eq) was added dropwise over 5 h maintaining the internal temperature at 110-115 ° C.The desired conversion was achieved 1 hour after the water addition was completed.The reaction mixture was cooled to 20 ° C and diluted with water (10 ml).The layers were separated and the aqueous layer re-extracted with toluene (20 ml).The combined organic layers were washed with 20 ml of 5percent w / w aqueous NaCl and then with 10percent w / w NaCl (40 ml) and finally with 20 ml of water.The resulting toluene solution was treated with activated carbon.After filtration, the filtrate was concentrated to dryness to give an orange oil (14 g).Cyclohexane (12 ml) was added at -5 / -10 ° C and the resulting suspension was filtered and washed twice with 3.5 ml of cyclohexane.The solid was dried under vacuum in a 25 ° C oven to give 10.8 g of a white solidbody.The molar yield after separation was 75percent. |
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