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Triethyl phosphite → HCID 22630503, compound

HRID 2416968
Notes
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Reaction equation

HRID 2416968 reaction equation
Br[CH2:2][CH2:3][CH2:4][CH2:5][C:6]([F:18])([F:17])[C:7]([F:16])([F:15])[C:8]([F:14])([F:13])[C:9]([F:12])([F:11])[F:10].[P:19]([O:26]CC)([O:23][CH2:24][CH3:25])[O:20][CH2:21][CH3:22]>>[CH2:21]([O:20][P:19]([CH2:2][CH2:3][CH2:4][CH2:5][C:6]([F:18])([F:17])[C:7]([F:16])([F:15])[C:8]([F:14])([F:13])[C:9]([F:12])([F:11])[F:10])([O:23][CH2:24][CH3:25])=[O:26])[CH3:22]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

3

Reactant 2

HCID 31215Triethyl phosphiteHCID 155453038-Bromo-1,1,1,2,2,3,3,4,4-nonafluorooctane

Product 1

HCID 22630503HCID 22630503, compoundYield 90.3%

Conditions

Temperature
150 °C

Procedure

A mixture of 12.40 g of 1-bromo-4-(nonafluorobutyl)butane and 21.00 g of triethyl phosphite was heated at 150° C. After 18 hr, diethyl ethylphosphonate and other volatiles were removed from the mixture by distillation, b.p. 30-50° C. at 0.05 torr (7 Pa). Bulb-to-bulb distillation of the remaining concentrated mixture provided 13.0 g of 1-(diethylphosphono)-4-(nonafluorobutyl)butane as a clear, colorless liquid, b.p. 105-110° C. at 0.05 torr (7 Pa).

Workup

  1. customdiethyl ethylphosphonate and other volatiles were removed from the mixture by distillation, b.p. 30-50° C. at 0.05 torr (7 Pa)
  2. distillationBulb-to-bulb distillation of the
  3. concentrationremaining concentrated mixture

Sources & evidence

ORD record
ord-dd129d79a6be4413b0ab3edafe345632
Source dataset
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06824882B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes