Method for preparation of chlorinated s-propylthiobarbituric acid
a technology of s-propylthiobarbituric acid and chlorinated s-propylthiobarbituric acid, which is applied in the field of preparation of chlorinated s-propylthiobarbituric acid, can solve the problems of serious environmental challenges and cost factors, and achieve the effects of reducing the number of sludge and sludge particles, and reducing the amount of sludg
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[0039]Compound of formula (3):
[0040]Compound of formula (4):
[0041]Compound of formula (5):
[0042]GC Method
[0043]Instrument:
[0044]Hewlett Packard gas chromatograph 6890 with a split injector and a flame ionisation detector or an instrument with corresponding performance and quality.
[0045]Column:
[0046]HP-1 (SIMDIST), 15 m×0.53 mm, 0.15 micrometer film-thickness, polydimethylsiloxane (or an equivalent column).
[0047]Instrument. Settings:
[0048]Oven:
INITIAL TEMP50°C.HOLD2minRAMP 120°C. / minNEXT TEMP320°C.HOLD10min
[0049]Injector:
Injection volume1 microliterCheck the auto-injector parameters
[0050]Inlets:
INJ. MODESplitINJ TEMP250°C.SPLIT FLOW200ml / minSPLIT RATIO25:1MODEconstant flow 8.0 ml / min
[0051]Detectors:
DET TEMP300° C.Check the FID gas flow rates
[0052]The GC results are given in area %.
example 1
[0069]5.0 g (21.62 mmol, 1 eq) compound of formula (1) were dissolved in 25 mL of DMF. 100 mL of DMF were mixed with 4.7 g of phosgene (47.56 mmol, 2.2 eq) at 0° C. The solution of compound of formula (1) was added to the mixture of DMF with phosgene at 0° C. After 14 h stirring at 0° C. and then 2 h at RT, 50 mL of water and 50 mL of toluene were added at 0° C. The mixture was stirred 15 min and the phases were separated. The organic phase was evaporated under vacuum. 5 g of compound of formula (2) were isolated (83% yield, 98.2% purity, GC analysis showed 1.1% of compound of formula (3), 0.32% of compound of formula (4) and 0.35% of compound of formula (5)).
example 2
[0070]50 g (216.2 mmol, 1 eq) of compound of formula (1) were dissolved in 250 mL of DMF. 1000 mL of DMF were mixed with 47 g of phosgene (475.6 mmol, 2.2 eq) at 0° C. The solution of compound of formula (1) was added to the mixture of DMF with phosgene at 0° C. After 14 h stirring at 0° C. and then 2 h at RT, 500 mL of water and 500 mL of toluene were added at 0° C. The mixture was stirred 30 min and the phases were separated. The organic phase was evaporated under vacuum. 54 g of compound of formula (2) were isolated (93% yield, 98.4% purity, GC analysis showed 1.1% of compound of formula (3), 0.26% of compound of formula (4) and 0.24% of compound of formula (5)).
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