Phosphorus oxide (P4O10) → 2,2,3,3-Tetrafluoro-3-iodopropanenitrile
反応式
[I:1][C:2]([C:5]([C:8]([NH2:10])=O)([F:7])[F:6])([F:4])[F:3].O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>>[I:1][C:2]([F:4])([F:3])[C:5]([F:7])([F:6])[C:8]#[N:10]参加物
3
反応条件
- 温度
- 140 °C
実験手順
A mixture of 150 g of fine powder of ICF2CF2CONH2 and 235 g of P2O5 was heated at 130 to 150° C., during which time volatiles were distilled out. Final volatiles were collected in a -78° C. trap at 26.6 kPa. A total of 125.3 g of crude product was obtained, 95% pure by GC. Redistillation gave pure product, bp 60-61° C. 19F NMR: -63.3 (t, J=10.4 Hz, 2F), -100.5 (t, J=10.4 Hz, 2F). IR(neat): 2264 (w), 1235 (s), 1196 (s), 1172 (s), 1146 (s), 1089 (s), 1065 (s), 893 (s).
後処理
- distillationwere distilled out
- customFinal volatiles were collected in a -78° C. trap at 26.6 kPa
出典と根拠
- ORDレコード
- ord-52882892903a46359ff83c3cf181eac6
- 出典データセット
- uspto-grants-2000_12
- 特許番号
- US06166157
反応ノート
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