Phosphorus oxide (P4O10) → HCID 131722241, compound

HRID 1276573Notes

Reaction equation

HRID 1276573 reaction equation
[I:1][C:2]([C:5]([O:11][C:12]([C:15]([C:18]([NH2:20])=O)([F:17])[F:16])([F:14])[F:13])([C:7]([F:10])([F:9])[F:8])[F:6])([F:4])[F:3].O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>>[I:1][C:2]([C:5]([O:11][C:12]([C:15]([C:18]#[N:20])([F:16])[F:17])([F:13])[F:14])([C:7]([F:10])([F:9])[F:8])[F:6])([F:4])[F:3]

Participants

3

Reactant 2

HCID 14812Phosphorus oxide (P4O10)HCID 131722242HCID 131722242, compound

Product 1

HCID 131722241HCID 131722241, compound

Conditions

Temperature
175 °C

Procedure

A mixture of 17.5 g of fine powder of ICF2CF(CF3)OCF2CF2CONH2 and 17 g of P2O5 was heated at 150 to 200° C., during which volatiles were distilled out. Final volatiles were collected in a -78° C. trap at 13.3 kPa. A total of 13.8 g of ICF2CF(CF3)OCF2CF2CN were obtained, 95% pure by GC. 19F NMR: -58.6 (dm J=212.4 Hz, 1F), -60.1 (dm J=212 Hz, 1F), -76.7 (m, 3F), -83.3 (dm, J=135 Hz, 1F), -84.8 (dm, J=135 Hz, 1F), -108.6 (t, j=6.3 Hz, 2F), -133.6 (m, 1F). IR(neat): 2268 (m), 1113 (s).

Workup

  1. distillationwere distilled out
  2. customFinal volatiles were collected in a -78° C. trap at 13.3 kPa

Sources & evidence

ORD record
ord-78f55ba59f2d45a79113f686bc2cb433
Source dataset
uspto-grants-2000_12
Patent number
US06166157

Reaction notes

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