2,2-Difluoroacetyl fluoride → 2,2-Difluoroacetyl chloride

Temperature

160 °C

A stainless steel reaction tube having an inner diameter of 23 mm and a length of 400 mm was packed with granular anhydrous calcium chloride (63 g, 120 cc; available from Junsei Chemical Co., Ltd. (particle size: about 2.5 to 3.5 mm)). While flowing nitrogen at 50 cc/min into the reaction tube, the reaction tube was heated at a setting temperature of 160° C. The flow of the nitrogen was stopped simultaneously with feeding the difluoroacetyl fluoride, which had been obtained in Raw Material Preparation Example 1, into the reaction tube at a rate of 0.3 g/min (retention time: 66 seconds). It was observed that a heat spot of 10 to 20° C. was generated in the vicinity of the inlet of the reaction tube and shifted toward the outlet of the reaction tube with the passage of time. The outlet gas was sampled and analyzed over time by the gas chromatograph. It was confirmed by the experimental results that difluoroacetyl chloride (DFAC) and difluoroacetyl fluoride (DFAF) were contained in the gas sample. The experimental results are graphed in FIG. 1.

1. customhad been obtained in Raw Material Preparation Example 1, into the reaction tube at a rate of 0.3 g/min (retention time: 66 seconds)
2. customwas observed that a heat spot of 10 to 20° C.
3. aliquotThe outlet gas was sampled

ORD record

ord-38fcbc7a4b93406ea06369d9f175fd18

Source dataset

uspto-grants-2014_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08716526B2