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Triethyl phosphite → 1-(Diethylphosphono)-1-(nonafluorobutyl)undecane

HRID 2416976
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HRID 2416976 반응식
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]([F:25])([F:24])[C:14]([F:23])([F:22])[C:15]([F:21])([F:20])[C:16]([F:19])([F:18])[F:17].[P:26]([O:33]CC)([O:30][CH2:31][CH3:32])[O:27][CH2:28][CH3:29]>>[CH2:28]([O:27][P:26]([CH:12]([C:13]([F:25])([F:24])[C:14]([F:23])([F:22])[C:15]([F:21])([F:20])[C:16]([F:19])([F:18])[F:17])[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH3:2])([O:30][CH2:31][CH3:32])=[O:33])[CH3:29]
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참가 물질

3

반응물 2

HCID 31215Triethyl phosphite2회HCID 2263051915-Bromo-1,1,1,2,2,3,3,4,4-nonafluoropentadecane

생성물 1

HCID 226305081-(Diethylphosphono)-1-(nonafluorobutyl)undecane수율 94.9%

반응 조건

온도
150 °C

실험 절차

A mixture of 15.03 g of 1-bromo-11-(nonafluorobutyl)undecane and 15.00 g of triethyl phosphite was heated at 150° C. After 18 hr, an additional 9.00 g of triethyl phosphite was added, and heating was continued for 24 hr. Diethyl ethylphosphonate and other volatiles were removed by distillation, b.p. 30-50° C. at 0.05 torr (7 Pa). Bulb-to-bulb distillation of the concentrate provided 16.07 g of 1-(diethylphosphono)-1-(nonafluorobutyl)undecane as a clear, colorless liquid, b.p. 170-200° C. at 0.05 torr (7 Pa).

후처리

  1. temperatureheating
  2. waitwas continued for 24 hr
  3. customDiethyl ethylphosphonate and other volatiles were removed by distillation, b.p. 30-50° C. at 0.05 torr (7 Pa)
  4. distillationBulb-to-bulb distillation of the concentrate

출처 및 근거

ORD 기록
ord-bf433777a2214835b90811356aab4a24
출처 데이터셋
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06824882B2

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