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4-TERT-BUTYL-PHENYLTHIOUREA synthesis

4synthesis methods
117174-73-9 Synthesis
N-BENZOYL-N'-[4-(TERT-BUTYL)PHENYL]THIOUREA

117174-73-9
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Yield:65259-90-7 81%

Reaction Conditions:

with sodium hydroxide in ethanol;Reflux;

Steps:

6.1 6.1 Preparation of N-(4-t-butylphenyl) thiourea

In a 100 mL round-bottomed flask, 12 mmol of benzoyl chloride and 20 mL of acetone were added.Then 12 mmol of potassium thiocyanate was added and a large amount of white solids were formed.After 15 minutes, the reaction is completed and the solid is filtered.The filtrate was spin-dry,The pale yellow liquid was taken directly into the next reaction.In a 100 mL round bottom flask, 10 mmol of 4-tert-butylaniline was added,30mL of ethyl acetate was dissolved and the product from the previous step was added to the solution.Heat to reflux reaction. After TLC tracks the reaction,The reaction solution was cooled to room temperature and the solvent was evaporated under reduced pressure.10 mL of ethanol and 10 mL of 2N sodium hydroxide solution were added directly and the reaction was refluxed.After TLC tracking reaction was completed, the reaction solution was cooled to room temperature and ice water (30 mL) was added.Neutralize with 2N hydrochloric acid.The solid was filtered to give the desired product as a light yellow solid, yield 81%.

References:

CN107629023,2018,A Location in patent:Paragraph 0172; 0173; 0174; 0175