Phosphorus oxide (P4O10) → HCID 131718531, compound

HRID 1728461Notes

Reaction equation

HRID 1728461 reaction equation
[C:1]([O:11][C:12]([C:18]([O:21][C:22]([C:31]([NH2:33])=O)([C:27]([F:30])([F:29])[F:28])[C:23]([F:26])([F:25])[F:24])([F:20])[F:19])([C:14]([F:17])([F:16])[F:15])[F:13])([C:4]([C:7]([F:10])([F:9])[F:8])([F:6])[F:5])([F:3])[F:2].O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>>[C:1]([O:11][C:12]([C:18]([O:21][C:22]([C:31]#[N:33])([C:27]([F:28])([F:29])[F:30])[C:23]([F:25])([F:26])[F:24])([F:19])[F:20])([C:14]([F:17])([F:16])[F:15])[F:13])([C:4]([C:7]([F:10])([F:9])[F:8])([F:6])[F:5])([F:3])[F:2]

Participants

3

Reactant 2

HCID 14812Phosphorus oxide (P4O10)HCID 131718530HCID 131718530, compound

Product 1

HCID 131718531HCID 131718531, compoundYield 94%

Procedure

A mixture of C3F7OCF(CF3)CF2OC(CF3)2CONH2 (3.81 g, 6.90 mmol) was heated with phosphorous pentoxide (9.02 g, 63.0 mmol) under nitrogen bypass at 214° C. for 3 hours. The distillate, collected during the heating period in 0° C. cooled receiver, was purified by fractionation in vacuum through traps held at -23°, -47°, -78°, and -196° C. The product, C3F7OCF(CF3)CF2OC(CF3)2CN, (3.42 g, 92% yield) VP0° C., 3 mmHg collected in the -23° and -47° C. traps was characterized by mass spectrometry. MS(70 eV) m/e (intensity, ion): 508 (2.7%, M-F), 458 (1.4%, M-C2F5), 342 (21.1%, M-C3F7O), 242 (33.9%, CF2OC(CF3)2CN), 192 (18.2%, OC(CF3)2CN), 176 (28.2%, C(CF3)2CN), 169 (100%, C3F7).

Workup

  1. distillationThe distillate, collected during the heating period in 0° C.
  2. temperaturecooled receiver
  3. customwas purified by fractionation in vacuum through traps
  4. customheld at -23°, -47°, -78°
  5. custom-196° C

Sources & evidence

ORD record
ord-c86db1a1d3da44a9a919e7fb62272d72
Source dataset
uspto-grants-1994_07
Patent number
US05326910

Reaction notes

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