1. Description
Crystalline Solid
https://www.echemi.com/
Basic Attributes
CAS No：931-86-2
Molecular Formula ：C3H4N4O
Molecular Mass ：112.09
Exact Mass ：112.038513
PSA ：79.8 A^2
LogP ：-1.2
EINECS ：213-242-9
InChIKeys ：MFEFTTYGMZOIKO-UHFFFAOYSA-N
H-bond Acceptor ：1
H-bond Donor ：2
SP3 ：0.00
RBN ：0
Characteristics
Density ：1.86
Melting Point ：>300 °C(lit.)
Flash Point ：258.1ºC
Refractive Index ：1.801
Storage Condition ：-20°C Freezer
BRN ：116378
Safety Information
2. HS Code ：2933699090
UN No. ：NONH for all modes of transport
WGK_Germany ：3
Risk Code ：20/21/22-36/37/38
Safety Instructions ：22-24/25-36-26
RTECS No. ：XZ2854300
Dangerous Mark ：Xi,Xn
P Code ：P301 + P312 + P330
Hazard Statements ：H302
Product Usage
Inhibits the growth of Escherichia coli
Production Methods
To 10L autoclave followed by anhydrous formic acid (99.5percent) 1.5Kg, Dicyandiamide 2.5 Kg
and p-toluenesulfonic acid catalyst (0.005 Kg). In sealed and stirred state, The reactor pressure
and slowly warmed to 110 , After the reaction, Slowly reduce the reaction temperature to room
temperature, A white solid was obtained.(2)The white solid was transferred to a 50 L glass
reaction kettle, Add 10L mass concentration of 5percent dilute hydrochloric acid.Heated to reflux
for 30 minutes until the solution becomes clear, The mixture was filtered through a filter
3. cartridge to the crystallizer, The filtrate was added 30percent aqueous ammonia in the crystallizer
to adjust the pH to 6, Precipitation of white crystals, After centrifugation, After drying in a hot air
oven, 5-azacytosine 2.8 kg (85percent yield based on dicyandiamide) was obtained.140 kg of
formic acid was charged into a reaction kettle, Turn on agitation, Twenty five kilograms of
dicyandiamide, The reaction temperature will gradually increase, Control temperature below 60 ,
The reaction temperature is no longer rising after the batch will be the remaining 75 kg of
dicyandiamide in 4 to 5 hours to join the reactor, The reaction temperature is controlled at 50 to
60 DEG C for 4 hours;Then stop the temperature control measures, The reaction temperature
increased slowly on its own, The temperature was raised to 100 to 110 ° C for 1 hour.120 kg of
acetic anhydride will drop into the reactor, During the dropping, the temperature was maintained
at 100 to 110 ° C, After dripping, And stirred at this temperature for 45 minutes;Again
dropping 100 kg of acetic anhydride, After dripping, Heating to reflux, The reflux reaction was
maintained for 2 hours.After refluxing, Stirring down to 60 ~ 70 , Adding 120 kg of ethanol, And
continued to cool to room temperature.filter, Filter cake into the reactor, 480 kg of ethyl acetate
and 96 kg of ethanol were added, Heated to 65 ~ 75 , After stirring for 1 hour, Filter cake drying,
Can be 5-azacytosine 74 kg, HPLC purity 98.9percentImpurity 1 content of 0.34percentImpurity 2
content of 0.06percent.
