[ CAS No. 116423-07-5 ] {[proInfo.proName]}

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2D 3D

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Quality Control of [ 116423-07-5 ]

COA NMR CNMR HPLC LC-MS

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SDS Specification

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Product Details of [ 116423-07-5 ]

CAS No. :	116423-07-5	MDL No. :	MFCD02628165
Formula :	C₈H₁₁NO₃	Boiling Point :	-
Linear Structure Formula :	-	InChI Key :	-
M.W :	169.18	Pubchem ID :	-
Synonyms :

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Application In Synthesis of [ 116423-07-5 ]

* 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.

Downstream synthetic route of [ 116423-07-5 ]

[ 116423-07-5 ] Synthesis Path-Downstream 1~9

1
[ 27428-42-8 ]
[ 116423-07-5 ]

Yield	Reaction Conditions	Operation in experiment
	With sodium hydroxide

Reference： [1]March [Annales de Chimie (Cachan, France), 1902, vol. <7> 26, p. 305][Comptes Rendus Hebdomadaires des Seances de l'Academie des Sciences, 1901, vol. 132, p. 697]

2
[ 116423-07-5 ]
[ 358721-54-7 ]

Yield	Reaction Conditions	Operation in experiment
	With oxalyl dichloride for 2h; Ambient temperature;
	With oxalyl dichloride; N,N-dimethyl-formamide In dichloromethane at 20℃; for 0.5h;	23 Oxalyl chloride (5.16 mL, 59.2 mmol) was added to a solution of β-(3,5-dimethyl-4-isoxazolyl)propionic acid (J. Org. Chem. 59(10); 1994; 2882) (2.5 g, 14.8 mmol) in dichloromethane (50 mL) and N,N-dimethylformamide (1 drop), and the solution was stirred at room temperature for 30 minutes. The mixture was concentrated under reduced pressure and the residue was azeotroped with dichloromethane (5×) to provide a brown liquid. This was dissolved in dichloromethane (25 mL), and tert-butyl carbazate (2.93 g, 22.2 mmol) was added portionwise. The mixture was diluted with further dichloromethane (23 mL) and the reaction was stirred for 18 hours at room temperature. The mixture was concentrated under reduced pressure, the residue was suspended in dichloromethane, the resulting precipitate was filtered off and the filtrate was evaporated under reduced pressure. The residue was purified by column chromatography on silica gel using an elution gradient of dichloromethane:methanol:0.88 ammonia (95:5:0.5 to 90:10:1) to provide the title compound as an oil, 3.08 g. 1H NMR (400 MHz, CDCl3): δ 1.45 (s, 9H), 2.21 (s, 3H), 2.36 (m, 4H), 2.45 (m, 1H), 2.60-2.73 (m, 2H), 6.48 (br s, 1H), 7.42 (br s, 1H). LCMS: m/z ES+306 [MNa]+

Reference： [1]Ceccherelli, Paolo; Curini, Massimo; Marcotullio, Maria Carla; Rosati, Ornelio; Wenkert, Ernest [Journal of Organic Chemistry, 1994, vol. 59, # 10, p. 2882 - 2884]
[2]Current Patent Assignee: PFIZER INC - US2005/154024, 2005, A1 Location in patent: Page/Page column 27-28

3
[ 154928-90-2 ]
[ 116423-07-5 ]