Silane, tris(1-methylethyl)- → CF3CF2CF2Ocf(CF3)cho

HRID 36465

반응식

HRID 36465 반응식
C([SiH](C(C)C)C(C)C)(C)C.[C:11]([C:15]([C:18]([O:21][C:22]([C:28](Cl)=[O:29])([C:24]([F:27])([F:26])[F:25])[F:23])([F:20])[F:19])([F:17])[F:16])([F:14])([F:13])[F:12]>[Pd]>[C:11]([C:15]([C:18]([O:21][C:22]([CH:28]=[O:29])([C:24]([F:26])([F:27])[F:25])[F:23])([F:20])[F:19])([F:17])[F:16])([F:14])([F:13])[F:12]

참가 물질

4

반응물 2

HCID 138754Silane, tris(1-methylethyl)-HCID 27825972,3,3,3-Tetrafluoro-2-(heptafluoropropoxy)propanoyl chloride

생성물 1

HCID 15717421CF3CF2CF2Ocf(CF3)cho수율 53.5%

시약·촉매·용매 1

HCID 23938Palladium촉매

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온도
0 °C

실험 절차

A 3-necked round bottom flask equipped with a dropping funnel and reflux condenser was charged with 10% Pd/C(0.35 g) and cooled to 0° C. Triisopropylsilane (6.0 g) was added. CF3CF2CF2OCF(CF3)COCl (10.9 g) was added, and the mixture was stirred at 25° C. for 75 hr. During this period, a total of 0.5 g of additional catalyst was added in ca. 0.1 g increments. Vacuum transfer and separation of the lower layer after chilling at -25° C. provided 5.26 g of liquid. 1H NMR (THF-d8 /F11): 9.9 (m). 19F NMR: -79.4 (m), -81.1 (s), -81.4 (t, J=7.2), -129.5 (s), -138.8 (m). 1H-decoupling experiment showed JHCCFCa. 2.5 Hz.

후처리

  1. customA 3-necked round bottom flask equipped with a dropping funnel
  2. temperaturereflux condenser
  3. waitDuring this period
  4. customVacuum transfer and separation of the lower layer
  5. temperatureafter chilling at -25° C.

출처 및 근거

ORD 기록
ord-1c4d85ecbe5f4908925f4e153def61fc
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05414140

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