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Triethyl phosphite → 1-(Diethylphosphono)-6-(nonafluorobutyl)hexane

HRID 2416965
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HRID 2416965 반응식
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][C:8]([F:20])([F:19])[C:9]([F:18])([F:17])[C:10]([F:16])([F:15])[C:11]([F:14])([F:13])[F:12].[P:21]([O:28]CC)([O:25][CH2:26][CH3:27])[O:22][CH2:23][CH3:24]>>[CH2:23]([O:22][P:21]([CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][C:8]([F:20])([F:19])[C:9]([F:18])([F:17])[C:10]([F:16])([F:15])[C:11]([F:14])([F:13])[F:12])([O:25][CH2:26][CH3:27])=[O:28])[CH3:24]
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참가 물질

3

반응물 2

HCID 31215Triethyl phosphite2회HCID 2263049110-Bromo-1,1,1,2,2,3,3,4,4-nonafluorodecane

생성물 1

HCID 226305161-(Diethylphosphono)-6-(nonafluorobutyl)hexane수율 91.1%

반응 조건

온도
150 °C

실험 절차

A mixture of 18.04 g of 1-bromo-6-(nonafluorobutyl)hexane and 19.6 g of triethyl phosphite was heated at 150° C. After 18 hr, an additional 10.0 g of triethyl phosphite was added, and heating was continued for 8 hr more. Diethyl ethylphosphonate and other volatiles were removed by distillation, b.p. 30-50° C. at 0.05 torr (7 Pa), and bulb-to-bulb distillation of the concentrate provided 18.88 g of 1-(diethylphosphono)-6-(nonafluorobutyl)hexane as a clear, colorless liquid, b.p. 120-130° C. at 0.05 torr (7 Pa).

후처리

  1. temperatureheating
  2. waitwas continued for 8 hr
  3. customDiethyl ethylphosphonate and other volatiles were removed by distillation, b.p. 30-50° C. at 0.05 torr (7 Pa), and bulb-to-bulb distillation of the concentrate

출처 및 근거

ORD 기록
ord-7f81d0f8f95f411ba8865a8ae6f5b201
출처 데이터셋
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06824882B2

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