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

HRID 3935

반응식

HRID 3935 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 23678859Sodium perfluorobutanoate수율 84%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-fdcb81caf14240578e9ddd54ada0a201
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04723016

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