Hexafluoropropylene → HCID 86641049、化合物

HRID 1479140ノート

反応式

HRID 1479140 の反応式
[OH:1][CH2:2][CH:3]1[CH2:7][O:6][C:5](=[O:8])[O:4]1.C(=O)([O-])[O-].[K+].[K+].[F:15][C:16]([F:23])([F:22])[C:17]([F:21])=[C:18]([F:20])[F:19]>C(#N)C>[F:19][C:18]([F:20])([O:1][CH2:2][CH:3]1[CH2:7][O:6][C:5](=[O:8])[O:4]1)[CH:17]([F:21])[C:16]([F:23])([F:22])[F:15]

参加物

5

反応条件

温度
45 °C

実験手順

Example 2 was prepared by combining 4-(hydroxymethyl)-1,3-dioxolan-2-one (100 g, 0.84 moles) (Huntsman, Salt Lake City, Utah) with potassium carbonate (23 g, 0.166 moles) and acetonitrile (200 mL) in a 600 mL Parr reactor. The reactor was warmed to 45° C. and hexafluoropropene (139 g, 0.92 moles) was added at a constant rate. The reactor was stirred until the decrease in pressure stopped. Volatile material was removed from the reaction mixture by rotary evaporation. The olefin of the desired product was present and was saturated by reaction with anhydrous HF at room temperature. Vacuum distillation was done to purify the product. The fraction that boiled at 145-150° C. at 3 T (0.4 kPa) was collected. The fraction was 97.5% pure. The product was analyzed by GC/MS and F-19 NMR. MCMB/LiFePO4 coin cells (2325) made and cycled as per Test Method E with Example 2 as the only electrolyte solvent had high impedance, and the capacity fade rate could not be calculated.

後処理

  1. customExample 2 was prepared
  2. customVolatile material was removed from the reaction mixture by rotary evaporation
  3. customwas saturated by reaction with anhydrous HF at room temperature
  4. distillationVacuum distillation
  5. customto purify the product
  6. customThe fraction that boiled at 145-150° C. at 3 T (0.4 kPa) was collected

出典と根拠

ORDレコード
ord-6759ec9667f24a2aa4e38652af74705d
出典データセット
uspto-grants-2016_08
特許番号
US09406977B2

反応ノート

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