1 3-PHENYLENE DIISOTHIOCYANATE 97 synthesis
- Product Name:1 3-PHENYLENE DIISOTHIOCYANATE 97
- CAS Number:3125-77-7
- Molecular formula:C8H4N2S2
- Molecular Weight:192.26
75-15-0
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108-45-2
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$13.00/25g
3125-77-7
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$140.00/1G
Yield:3125-77-7 91.3%
Reaction Conditions:
Stage #1: carbon disulfide;m-phenylenediaminewith potassium carbonate in dichloromethane;water at 0 - 10; for 1 h;
Stage #2: with 1,3,5-trichloro-2,4,6-triazine in dichloromethane at 0 - 10; for 0.5 h;
Steps:
4 Preparation of m-phenylisothiocyanate (Intermediate 1)
10 ml of CS2 was added to a solution of m-phenylenediamine (3. 0 g, 27.74 mmol) in 20 ml of DCM and potassium carbonate (7. 66 g, 55.48 mmol) in water (20 ml) under ice-cooling. The mixture was stirred at 0 to 10 ° C for 1 hour.10 ml DCM was added,3. 5 grams of cyanuric chloride (18. 5 mmol) of solid powder,0-10 degrees Celsius stirring 30 minutes,Room temperature 3-5 hours,0-10 degrees Celsius dropping 6N sodium hydroxide adjusted pH = 11.The organic phase was separated and the aqueous phase was extracted with dichloromethane (15 ml x 3). The organic phases were combined and dried over anhydrous sodium sulfate. The filtrate was concentrated and purified by silica gel column chromatography (petroleum ether: dichloromethane = 9: 1) Yielding 4.87 g of intermediate 1 in 91.3% yield.
References:
CN104529876,2016,B Location in patent:Paragraph 0075-0079
463-71-8
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108-45-2
480 suppliers
$13.00/25g
3125-77-7
30 suppliers
$140.00/1G
19972-68-0
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3125-77-7
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$140.00/1G
108-45-2
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$13.00/25g
102368-13-8
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$13.00/1g
3125-77-7
30 suppliers
$140.00/1G
108-45-2
480 suppliers
$13.00/25g
3125-77-7
30 suppliers
$140.00/1G