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CAS RN: 430-67-1 | 产品编码: D4758
2,2-Difluoroethylamine
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技术规格
| Appearance | Colorless to Yellow clear liquid |
| Purity(GC) | min. 98.0 % |
| Purity(Neutralization titration) | min. 98.0 % |
| NMR | confirm to structure |
物性（参考值）
| 沸点 | 68 °C |
| 闪点 | -34 °C |
| 比重 | 1.17 |
| 折射率 | 1.34 |
GHS
| 象形图 |
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| 信号词 | Danger |
| 危险性说明 | H314 : Causes severe skin burns and eye damage. H225 : Highly flammable liquid and vapor. |
| 防范说明 | P501 : Dispose of contents/ container to an approved waste disposal plant. P240 : Ground/bond container and receiving equipment. P210 : Keep away from heat/sparks/open flames/hot surfaces. No smoking. P233 : Keep container tightly closed. P243 : Take precautionary measures against static discharge. P241 : Use explosion-proof electrical/ ventilating/ lighting/ equipment. P242 : Use only non-sparking tools. P264 : Wash skin thoroughly after handling. P280 : Wear protective gloves/ protective clothing/ eye protection/ face protection. P370 + P378 : In case of fire: Use dry sand, dry chemical or alcohol-resistant foam to extinguish. P303 + P361 + P353 : IF ON SKIN (or hair): Take off immediately all contaminated clothing. Rinse skin with water/shower. P301 + P330 + P331 : IF SWALLOWED: Rinse mouth. Do NOT induce vomiting. P363 : Wash contaminated clothing before reuse. P304 + P340 + P310 : IF INHALED: Remove person to fresh air and keep comfortable for breathing. Immediately call a POISON CENTER/doctor. P305 + P351 + P338 + P310 : IF IN EYES: Rinse cautiously with water for several minutes. Remove contact lenses, if present and easy to do. Continue rinsing. Immediately call a POISON CENTER/doctor. P403 + P235 : Store in a well-ventilated place. Keep cool. P405 : Store locked up. |
相关法规
运输信息
| UN编号 | UN2733 |
| 类别 | 3 / 8 |
| 包装类别 | II |
| HS编码* | 2921.19-000 |
应用
Reagents for Difluoromethylation (Precursor to difluoromethyl diazomethane)
Typical Procedure:
To a stirred solution of 2,2-difluoroethylamine (193 mg, 2.38 mmol, 2.0 eq.) in CHCl3 (20 mL), tert-butyl nitrite (294 mg, 2.86 mmol, 2.4 eq.) and acetic acid (28 mg, 0.48 mmol, 0.4 eq.) are added. The solution is heated at reflux whereas the mixture becomes deeply yellow. After 10 min, the heating is stopped, and the reaction mixture is cooled down to a room temperature by external water bath. Methyl propiolate (100 mg, 1.19 mmol, 1.0 eq.) is added at once. The reaction mixture is left at room temperature for 24 h. The solvent is evaporated under vacuum. The formed oily residue is purified by column chromatography on silica gel using hexane-EtOAc (2:1) as an eluent, to afford the pure product (159 mg, 0.90 mmol, 76% yield) as a colorless solid.
To a stirred solution of 2,2-difluoroethylamine (193 mg, 2.38 mmol, 2.0 eq.) in CHCl3 (20 mL), tert-butyl nitrite (294 mg, 2.86 mmol, 2.4 eq.) and acetic acid (28 mg, 0.48 mmol, 0.4 eq.) are added. The solution is heated at reflux whereas the mixture becomes deeply yellow. After 10 min, the heating is stopped, and the reaction mixture is cooled down to a room temperature by external water bath. Methyl propiolate (100 mg, 1.19 mmol, 1.0 eq.) is added at once. The reaction mixture is left at room temperature for 24 h. The solvent is evaporated under vacuum. The formed oily residue is purified by column chromatography on silica gel using hexane-EtOAc (2:1) as an eluent, to afford the pure product (159 mg, 0.90 mmol, 76% yield) as a colorless solid.
References
- In Situ Generation of Difluoromethyl Diazomethane for [3+2] Cycloadditions with Alkynes
参考文献
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