4,4,5,5,6,6,7,7,7-Nonafluoroheptanenitrile → HCID 22013473, compound

Temperature

110 °C

A 210-ml shaker tube was charged with 30 g of C4F9CH2CH2CN, 4.0 g of PtB on activated carbon (2%) and 30 ml THF. The vessel was closed, cooled, evacuated and pressured with hydrogen to 3.5 MPa. The vessel was heated to 110° C. and hydrogen pressure was adjusted to 10.3 MPa. The mixture was shaken for 16 h. The vessel was cooled and the gas was vented slowly. The contents were filtered and the filtrate was distilled to remove THF. The residue was distilled at reduced pressure to give 4,4,5,5,6,6,7,7,7-nonafluoroheptylamine (4.0 g, 13%, b.p. 94-97° C./24 kPa absolute) and di(4,4,5,5,6,6,7,7,7-nonailuoroheptyl)amine (20.5 g, 69%, b.p. 105-108° C./270 Pa absolute). The distillation residue (0.2 g) was mainly (C4F9CH2CH2CH2)3N.

1. customThe vessel was closed
2. temperaturecooled
3. customevacuated
4. temperatureThe vessel was cooled
5. filtrationThe contents were filtered
6. distillationthe filtrate was distilled
7. customto remove THF
8. distillationThe residue was distilled at reduced pressure

ORD record

ord-866895660b7147d3ad3492cec1773528

Source dataset

uspto-grants-2000_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06054615