Methyl 2,2,3,3,4,4,4-heptafluorobutanoate → Sodium perfluorobutanoate

HRID 3935

反応式

HRID 3935 の反応式
[F:1][C:2]([F:14])([C:7]([F:13])([F:12])[C:8]([F:11])([F:10])[F:9])[C:3]([O:5]C)=[O:4].C[Si](C)(C)[O-].[Na+:20]>CCOCC>[F:1][C:2]([F:14])([C:7]([F:12])([F:13])[C:8]([F:9])([F:10])[F:11])[C:3]([O-:5])=[O:4].[Na+:20]

参加物

4

反応物 2

HCID 67741Methyl 2,2,3,3,4,4,4-heptafluorobutanoateHCID 23672319Sodium trimethylsilanolate

生成物 1

HCID 23678859Sodium perfluorobutanoate収率 84%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

Methyl perfluorobutyrate (12.81 g, 56 mmol) was added dropwise to a stirred solution of sodium trimethylsilanolate (6.3 g, 56 mmol) in dry ether (300 mL) at room temperature under nitrogen. The reaction mixture was stirred overnight. The solid was filtered under nitrogen, washed with dry ether, and dried under a stream of nitrogen to afford sodium perfluorobutyrate (11.1 g, 84% yield) as a white solid: 19F NMR (D2O) δ -79.6 (t, J=8 Hz, CF3 --, 3F), -117.2 (q, J=8 Hz, CF3CF2CF2 --, 2F), -126.2 ppm (s, CF3CF2 --, 2F). Anal. Calcd. for C4F7NaO2 : C, 20.36; F, 56.35; Na, 9.74. Found: C, 20.84, 20.61, 20.58; F, 56.68, 53.24; Na, 9.89, 9.65.

後処理

  1. filtrationThe solid was filtered under nitrogen
  2. washwashed with dry ether
  3. customdried under a stream of nitrogen

出典と根拠

ORDレコード
ord-fdcb81caf14240578e9ddd54ada0a201
出典データセット
uspto-grants-1988_02
特許番号
US04723016

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