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Sodium Hydroxide → HCID 19063467, compound

HRID 267650
Notes
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Reaction equation

HRID 267650 reaction equation
[F:1][C:2]([F:11])([C:7]([F:10])([F:9])[F:8])[CH2:3][O:4][CH2:5]Cl.Br(F)(F)[F:13].[OH-].[Na+]>>[F:1][C:2]([F:11])([C:7]([F:10])([F:9])[F:8])[CH2:3][O:4][CH2:5][F:13]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

3

Reactant 2

HCID 14798Sodium HydroxideHCID 215171363-(Chloromethoxy)-1,1,1,2,2-pentafluoropropane

Product 1

HCID 19063467HCID 19063467, compound

Conditions

Temperature
-5 °C

Procedure

The ether XXVII was refractionated to obtain a sample (56.8 g, 0.286 mole) of <99% purity by GLC. This sample was cooled to -5°C and stirred in a teflon bottle as bromine trifluoride (15.6 g, 0.114 mole) was added dropwise. The product was stirred with ice and dilute sodium hydroxide solution to remove halogens and acids, separated, washed with distilled water, freeze-dried at -20°C and then dried at 0°C over type 3A molecular sieve. The V so obtained was 99.0% by GLC; micro b760 62.2°C; d42 1.41; yield 45 g (87% of theory). The molecular sieve type 3A is manufactured and sold by the Linde Division of Union Carbide Company.

Workup

  1. customto obtain a sample (56.8 g, 0.286 mole) of <99% purity by GLC
  2. additionwas added dropwise
  3. customto remove halogens and acids
  4. customseparated
  5. washwashed with distilled water
  6. customfreeze-dried at -20°C
  7. dry with materialdried at 0°C over type 3A molecular sieve
  8. customThe V so obtained
  9. custommicro b760 62.2°C

Sources & evidence

ORD record
ord-6bd1a3a8350f454dad812ab9edeabe5d
Source dataset
uspto-grants-1976_03
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US03943256

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes