Sodium borohydride → Tris(pentafluoroethyl)phosphane
Reaction equation
F[P:2](F)([C:17]([F:23])([F:22])[C:18]([F:21])([F:20])[F:19])([C:10]([F:16])([F:15])[C:11]([F:14])([F:13])[F:12])[C:3]([F:9])([F:8])[C:4]([F:7])([F:6])[F:5].[BH4-].[Na+]>>[F:9][C:3]([P:2]([C:10]([F:15])([F:16])[C:11]([F:12])([F:13])[F:14])[C:17]([F:23])([F:22])[C:18]([F:21])([F:20])[F:19])([F:8])[C:4]([F:7])([F:6])[F:5]Participants
Conditions
- Temperature
- 110 °C
Procedure
230.0 g (0.54 mol) of difluorotris(pentafluoroethyl)phosphorane and 41.2 g (1.089 mol) of sodium borohydride were refluxed with vigorous stirring for 3 hours in a glass flask at a bath temperature of about 110° C. The reaction mixture was subsequently distilled under reduced pressure (2 kPa), and two fractions of the product were collected in cold traps at a temperature of −78° C. and −195° C. respectively. For further purification, the combined products from both traps were distilled under atmospheric pressure under an inert-gas atmosphere, with the fraction in the boiling range 85-87° C. being collected. 194.0 g of pure tris(pentafluoroethyl)phosphine were obtained. The yield was 93%, based on the amount of difluorotris(pentafluoroethyl)phosphorane employed. The resultant product was characterised by means of 19F- and 31P-NMR spectroscopy. The chemical shifts found correspond to those from Example 1a.
Workup
- distillationThe reaction mixture was subsequently distilled under reduced pressure (2 kPa), and two fractions of the product
- customwere collected in cold traps at a temperature of −78° C. and −195° C. respectively
- customFor further purification
- distillationthe combined products from both traps were distilled under atmospheric pressure under an inert-gas atmosphere, with the fraction in the boiling range 85-87° C.
- custombeing collected
Sources & evidence
- ORD record
- ord-16277ba517594e568a5dcf6c776741ed
- Source dataset
- uspto-grants-2009_12
- Patent number
- US07632969B2
Reaction notes
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