ChemicalBook CAS DataBase List N-METHOXY-N-METHYLTRIFLUOROACETAMIDE

N-METHOXY-N-METHYLTRIFLUOROACETAMIDE synthesis

5synthesis methods

Product Name:N-METHOXY-N-METHYLTRIFLUOROACETAMIDE
CAS Number:104863-67-4
Molecular formula:C4H6F3NO2
Molecular Weight:157.09

6638-79-5

407-25-0

104863-67-4

To a suspension of N,O-dimethylhydroxylamine hydrochloride (107.2 kg, 1.1 kmol) in dichloromethane (400 L) was sequentially added trifluoroacetic anhydride (210 kg, 1 kmol) and pyridine (174 kg, 2.2 kmol) at 0 °C. The reaction mixture was stirred continuously at 0 °C for 1 hour. Subsequently, the reaction solution was diluted with ice water (300 L) and washed with 2M hydrochloric acid (300 L). The aqueous phase was extracted twice with dichloromethane, the organic phases were combined and dried with anhydrous magnesium sulfate. After concentration of the organic phase, the crude N-methoxy-N-methyl-2,2,2-trifluoroacetamide (Weinreb amide) was obtained with 90% purity and 95% yield, which could be used in the subsequent reaction without further purification.

6638-79-5 Synthesis

6638-79-5
595 suppliers
$6.00/25g

407-25-0 Synthesis

407-25-0
473 suppliers
$9.00/1g

104863-67-4
149 suppliers
$5.00/250mg

Yield:104863-67-4 95%

Reaction Conditions:

with pyridine in dichloromethane at 0; for 1 h;Large scale;

Steps:

General procedure

To a suspension of N,O-dimethyl-hydroxylamine hydrochloride (107.2 Kg, 1.1 kmol) in dichloromethane (400 L) were added trifluoroacetic anhydride (210 Kg, 1 kmol) and pyridine (174 Kg, 2.2 kmol) sequentially at0 °C. The mixture was stirred at 0°C for 1 h and then diluted with ice water (300 L) and washed with 2 M HCl (300 L). The aqueous solution was extracted twice with dichloromethane and dried under MgSO4. The crude Weinreb amide was obtained after concentration without further purification (90 %purity, 95 % yield).

References:

Jiang;Cheng;Yuan [Asian Journal of Chemistry,2015,vol. 27,# 7,p. 2406 - 2408]

6638-79-5 Synthesis

6638-79-5
595 suppliers
$6.00/25g

104863-67-4
149 suppliers
$5.00/250mg

References

6638-79-5 Synthesis

6638-79-5
595 suppliers
$6.00/25g

76-05-1 Synthesis