ChemicalBook CAS DataBase List 3-THIOPHENECARBOXYLIC ACID HYDRAZIDE

3-THIOPHENECARBOXYLIC ACID HYDRAZIDE synthesis

4synthesis methods

Product Name:3-THIOPHENECARBOXYLIC ACID HYDRAZIDE
CAS Number:39001-23-5
Molecular formula:C5H6N2OS
Molecular Weight:142.18

5751-80-4 Synthesis

5751-80-4
140 suppliers
$6.00/1g

39001-23-5
53 suppliers
$32.00/250mg

Yield:39001-23-5 100%

Reaction Conditions:

with hydrazine in ethanol;Heating / reflux;

Steps:

A solution of ethyl-3-thiophene carboxylate (2 g, 12.8 mmol) and hydrazine monohydrate (6.2 ml, 128 mmol) in EtOH (10 ml) was refluxed overnight. The mixture was concentrated to dryness to afford intermediate 1 (1.86 g, 100%). A portion of this material (500 mg) was dissolved in acetone (5 ml) and the solution was heated to 60° C. overnight. The solution was concentrated to dryness. The residue was dissolved in TFA (5 ml) and treated with triethylsilane (1.16 ml, 7.24 mmol) at 60° C. overnight. The reaction mixture was concentrated under reduced pressure and the residue was partitioned between saturated aqueous bicarbonate and DCM. The organic layer was washed with brine, dried over sodium sulfate and concentrated under vacuum to afford the product as a white solid (484 mg, 75%).

References:

US2006/178532,2006,A1 Location in patent:Page/Page column 9 US2006/258740,2006,A1 Location in patent:Page/Page column 9

22913-26-4 Synthesis