2 4-TOLYLENE DIISOTHIOCYANATE 97 synthesis

6synthesis methods

Product Name:2 4-TOLYLENE DIISOTHIOCYANATE 97
CAS Number:4891-66-1
Molecular formula:C9H6N2S2
Molecular Weight:206.29

75-15-0
248 suppliers
$40.00/100g

95-80-7 Synthesis

95-80-7
256 suppliers
$12.00/1mg

4891-66-1
10 suppliers
$126.00/5g

Yield:4891-66-1 78.5%

Reaction Conditions:

Stage #1: carbon disulfide;4-methylbenzene-1,3-diaminewith potassium carbonate in dichloromethane;water; for 1 h;Cooling with ice;
Stage #2: with 1,3,5-trichloro-2,4,6-triazine in dichloromethane;water at 20; for 3.5 h;Cooling with ice;
Stage #3: with sodium hydroxide in dichloromethane;water at 0 - 10; pH=11;

Steps:

3.2 Preparation of 2,2,4-toluene diisothiocyanate (Intermediate 1):

12 ml of carbon disulfide was added to 2.0 g (16.37 mmol) of 2,4-diaminotoluene in an ice-water bath15 ml of DCM and 4.75 g of K2CO3 (34.38 mmol) in 15 ml of water was stirred for 1 hour. Cyanuric chloride 2.05 g(10.92 mmol) and 15 ml of DCM were successively added to the reaction system and the stirring was continued for 30 minutes in an ice-water bath and allowed to warm to room temperature for 3 hours. willThe reaction system again cooled to 0-10 degrees Celsius, dropping 6M NaOH aqueous solution, adjust the pH = 11. At 0 degrees Celsius stirring 1 smallThe organic phase was separated and the aqueous phase was extracted twice with dichloromethane. The organic phases were combined, dried over anhydrous Na2SO4, filtered and concentrated.Petroleum ether as a mobile phase silica gel column to give 2.37 g of a colorless oily compound in a yield of 78.5%.

References:

CN104529875,2017,B Location in patent:Paragraph 0053; 0054; 0055; 0056; 0057

584-84-9 Synthesis