Chemical Products 5-Azacytosine Production Methods

Chemical Products 5-Azacytosine Description
Crystalline Solid

Chemical Products 5-Azacytosine 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

Chemical Products 5-Azacytosine Characteristics
Density ：1.86

Melting Point ：>300 °C(lit.)

Flash Point ：258.1ºC

Refractive Index ：1.801

Storage Condition ：-20°C Freezer

BRN ：116378

Chemical Products 5-Azacytosine Safety Information
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

Chemical Products 5-Azacytosine Product Usage
Inhibits the growth of Escherichia coli

Chemical Products 5-Azacytosine 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 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.

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