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ChemicalBook CAS DataBase List Carbamic acid, N-[4-(difluoromethyl)-2-thiazolyl]-, 1,1-dimethylethyl ester
947179-19-3

Carbamic acid, N-[4-(difluoromethyl)-2-thiazolyl]-, 1,1-dimethylethyl ester synthesis

3synthesis methods
494769-34-5 Synthesis
(4-FORMYLTHIAZOL-2-YL)CARBAMIC ACID TERT-BUTYL ESTER

494769-34-5
97 suppliers
$50.00/250mg

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Yield:947179-19-3 60%

Reaction Conditions:

Stage #1: (4-formyl-thiazol-2-yl)-carbamic acid tert-butyl esterwith diethylamino-sulfur trifluoride in dichloromethane at 20; for 16 h;
Stage #2: with sodium hydrogencarbonate in dichloromethane;water;

Steps:

89.1 Step 1:

Step 1: (4-Difluoromethylthiazol-2-yl)-carbamic acid tert-butyl ester To a solution of 1.25 g (5.5 mmol) (4-formyl-thiazol-2-yl)-carbamic acid tert-butyl ester (CAS: [494769-34-5]) in 30 ml of dry methylene chloride were added 2.15 ml (16.4 mmol) diethylaminosulfur trifluoride (DAST). The mixture was stirred at room temperature for 16 hours. The reaction mixture was quenched with sat. NaHCO3- solution and extracted with water and methylene chloride. The combined organic extracts were dried with sodium sulfate, filtered and evaporated. The crude product was purified by flash chromatography on silica gel (heptane/ethyl acetate 4:1). The desired compound was obtained as a yellow solid (810 mg, 60%), MS: m/e=251.2 (M+H)+.

References:

US2007/197553,2007,A1 Location in patent:Page/Page column 28