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Type | HazMat fee for 500 gram (Estimated) |
Excepted Quantity | USD 0.00 |
Limited Quantity | USD 15-60 |
Inaccessible (Haz class 6.1), Domestic | USD 80+ |
Inaccessible (Haz class 6.1), International | USD 150+ |
Accessible (Haz class 3, 4, 5 or 8), Domestic | USD 100+ |
Accessible (Haz class 3, 4, 5 or 8), International | USD 200+ |
CAS No. : | 5394-63-8 | MDL No. : | MFCD00040468 |
Formula : | C7H10O3 | Boiling Point : | - |
Linear Structure Formula : | CH3COC(CH3)2OCOCH | InChI Key : | XFRBXZCBOYNMJP-UHFFFAOYSA-N |
M.W : | 142.15 | Pubchem ID : | 79368 |
Synonyms : |
Signal Word: | Danger | Class: | 3 |
Precautionary Statements: | P501-P260-P202-P240-P210-P233-P201-P243-P241-P242-P264-P280-P370+P378-P308+P313-P337+P313-P305+P351+P338-P362+P364-P303+P361+P353-P332+P313-P403+P235-P405 | UN#: | 1993 |
Hazard Statements: | H315-H319-H361-H373-H225 | Packing Group: | Ⅱ |
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 |
---|---|---|
Sodium hydroxide (1.06 g, 26. 5 mmol) was added to a solution of <strong>[24835-08-3]2-nitrobenzylamine hydrochloride</strong> (5.0 g, 26.5 mmol) in a mixed solvent comprising 20 ml of methanol and 2 ml of water, followed by stirring at room temperature for 30 minutes. Then, the reaction solution was concentrated under reduced pressure, toluene was added to the resulting residue, followed by azeotropic water separation under reduced pressure to distill the solvent off. To the resulting residue, 100 ml of m-xylene and 2,2,6-trimethyl-1,3-dioxin-4-one (3.77 g, 26.5 mmol) were added, followed by reflux under heating with stirring for 1 hour with azeotropic water separation with a dean-stark apparatus. After the reaction, ethyl acetate and water were added, and the organic layer was separated, dried with saturated aqueous sodium chloride and over anhydrous sodium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (n-hexane/ethyl acetate=9/1 to 1/1) to obtain 2.27 g of the desired product. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
31% | In 5,5-dimethyl-1,3-cyclohexadiene; for 4h;Reflux; Inert atmosphere; | To a solution of Boc-amino acetone3 17 (4.21 g, 24.3 mmol) in xylenes (24 mL) was added 2,2,6-trimethyl-4H-1,3-dioxin-4-one 18 (7.1 mL, 48.6 mmol). The reaction was heated to reflux (130 C) for 4 h, was cooled to 23 C and concentrated under reduced pressure to afford crude beta-ketoamide. Purification by flash column chromatography (CH2Cl2:Et2O 90:10) provided mixed fractions of beta-ketoamide and alpha,beta-unsaturated lactam 19. alpha,beta-Unsaturated lactam 19 was isolated (1.37, 24%) as a yellow oil. The mixed fractions were re-subjected to flash column chromatography (CH2Cl2:Et2O 90:10) which provided alpha,beta-unsaturated lactam 19 (1.78 g, 31%) for a combined yield of 3.15 g (55%) of a yellow oil. To a solution of alpha,beta-unsaturated lactam 19 (1.40 g, 6.0 mmol) in toluene (120 mL) was added DIBAL-H in hexanes (12 mL, 1.0 M solution, 12 mmol) at -78 C. The reaction was stirred for 4 h, quenched with EtOAc (10 mL)and Rochelle?s salt (20 mL) at -78 C, and allowed to warm to 23 C while stirring vigorously overnight. The solution was diluted with CH2Cl2 (300 mL) and poured over Celite. The organic extracts were separated and washed with brine (60 mL), dried over Na2SO4, decanted, and concentrated under reduced pressure. Purification by flash column chromatography (hexanes:EtOAc 40:60) delivered allylic alcohol (408 mg, 28%) as an orange oil. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
31% | In para-xylene; at 150℃; for 4h;Inert atmosphere; | From Boc-aminoacetone 42: To a solution of Boc-aminoacetone 42(4.21 g, 24.3 mmol) in p-xylene (24 mL) was added dioxinone 43 (7.1mL, 48.6 mmol). The reaction was heated to reflux (150 C) for 4 h,cooled to 23 C, and concentrated under reduced pressure to afford the crude beta-keto amide. Purification by flash column chromatography (CH2Cl2-Et2O, 90:10) provided mixed fractions of beta-keto amideand unsaturated Boc-lactam 40. Unsaturated Boc-lactam 40was isolated (1.37 g, 24%) as a yellow oil. The mixed fractions were re-introduced to flash column chromatography (CH2Cl2-Et2O, 90:10), whichprovided an additional amount of lactam 40(1.78 g, 31%) as a yellow oil; combined total yield: 3.15 g (55%). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
99% | In 5,5-dimethyl-1,3-cyclohexadiene; at 150℃; for 0.166667h;Inert atmosphere; | To a round-bottomed flask was added 42 (10.6 g, 61.0 mmol), dioxinone 43 (8.9 mL, 61.0 mmol), and xylenes (61 mL), and heated to 150 C for 10 min. The reaction was allowed to cool and the mixture was concentrated under reduced pressure to give beta-keto amide 41 as a brown solid; yield: 15.54 g (60.4 mmol, 99%). |
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