372-29-2
Ethyl 3-amino-4,4,4-trifluorocrotonate
CAS: 372-29-2
Molecular Formula: C6H8F3NO2
372-29-2 - Names and Identifiers
372-29-2 - Physico-chemical Properties
| Molecular Formula | C6H8F3NO2 |
| Molar Mass | 183.13 |
| Density | 1.245g/mLat 25°C(lit.) |
| Melting Point | 26°C |
| Boling Point | 83°C15mm Hg(lit.) |
| Flash Point | 149°F |
| Solubility | Chloroform (Slightly), Methanol (Slightly) |
| Vapor Presure | 1.16mmHg at 25°C |
| Appearance | Colourless to Pale Yellow Low-Melting to Semi-Solid |
| Color | White or Colorless to Light yellow |
| BRN | 4397839 |
| pKa | 0.76±0.70(Predicted) |
| Storage Condition | 2-8°C(protect from light) |
| Sensitive | Air Sensitive |
| Refractive Index | n20/D 1.424(lit.) |
372-29-2 - Risk and Safety
| Risk Codes | R20/21/22 - Harmful by inhalation, in contact with skin and if swallowed. R36/37 - Irritating to eyes and respiratory system. |
| Safety Description | S26 - In case of contact with eyes, rinse immediately with plenty of water and seek medical advice. S36 - Wear suitable protective clothing. S36/37 - Wear suitable protective clothing and gloves. |
| UN IDs | 3259 |
| WGK Germany | 3 |
| HS Code | 29224999 |
| Hazard Note | Toxic/Irritant |
| Hazard Class | 8 |
372-29-2 - Reference Information
| freezing point | 22.0 to 26.0 ℃ |
| properties | 3-amino -4,4, 4-trifluorocrotonate ethyl ester is a colorless liquid at room temperature, boiling point 175.3 ℃ (normal pressure),83 ℃(15mmHg), flash point 59.8 ℃, relative density 1.245, refractive index 1.424. |
| application | 3-amino -4,4, 4-trifluorocrotonate ethyl ester is an active intermediate in the synthesis of pesticides, medicines and other industrial chemicals, especially suitable for the preparation of trifluoromethyl substituted heterocyclic compounds, such as uracil derivatives, thiazole derivatives, oxazine derivatives and pyridine derivatives. |
| preparation | amination reactor volume is 1000L, equipped with stirring, thermometer, metering tank and condenser. 368.0kg(2.0kmol)4,4, 4-trifluoroacetoacetate was added into the reactor through the metering tank, and the temperature was raised to 90 ℃. Then 323.4kg(4.2kmol) of ammonium acetate is put in and kept at 90 ℃ for 3 hours. Cool the reaction solution to 30 ℃, stop stirring and let stand for 30 minutes. The reaction solution is divided into two layers, the lower layer is organic phase, the weight is 359.6kg, the content of 3-amino -4,4,4-trifluorocrotonate ethyl ester is 98.2%, the yield is 96.5%; the upper layer is water phase, the water phase weighs 330.6kg, and the content of acetic acid in the water phase is 36.3%. The resulting 359.6kg aqueous phase was transferred to a 1000L neutralization reactor equipped with stirring, thermometer, metering tank and condenser. After stirring is turned on, the temperature is raised to 40 ℃ and then 20% ammonia water is added dropwise, and the dropwise dosage is 204.0kg (equivalent to 1.2 equivalents of acetic acid). After dropping, the temperature of the system is increased to 70 ℃, and the water and excess ammonia in the system are removed at a vacuum degree of-95KPa. Finally, 318.2kg of white ammonium acetate solid was obtained with a purity of 98.2% and a recovery rate of 96.6%. |
Last Update：2024-04-10 22:29:15
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