Ethylene Glycol → HCID 178506434, compound

HRID 1766632Notes

Reaction equation

HRID 1766632 reaction equation
[F:1][P-:2]([F:7])([F:6])([F:5])([F:4])[F:3].F[C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:16]=[CH:17][CH:18]=[C:19]3[C:28]=2[S:27][C:26]2[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=2[SH+:20]3)=[CH:11][CH:10]=1.[CH2:29]([OH:32])[CH2:30][OH:31].[OH-].[K+].O>ClCCl>[F:1][P-:2]([F:7])([F:6])([F:5])([F:4])[F:3].[OH:31][CH2:30][CH2:29][O:32][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:16]=[CH:17][CH:18]=[C:19]3[C:28]=2[S:27][C:26]2[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=2[SH+:20]3)=[CH:11][CH:10]=1

Participants

6

Reactant 4

HCID 174Ethylene GlycolHCID 962WaterHCID 14797Potassium HydroxideHCID 178506433HCID 178506433, compound

Product 1

HCID 178506434HCID 178506434, compoundYield 92%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Conditions

Temperature
120 °C

Procedure

A round bottom flask was charged with 0.2 g (0.438 mmol) of 9-(4-fluoro-phenyl)-thianthrenium hexafluorophosphate, and 5.0 g of ethylene glycol. The mixture was heated up to 120° C. and stirred until complete dissolution. 50 mg of potassium hydroxide were added to this solution; the solution was stirred for 1 hour and then poured into water. Dichloromethane was added and the organic layer separated, washed with water and dried (Na2SO4). After drying the solvent was removed under vacuum to give a white solid (0.2 g, 92%).

Workup

  1. stirringthe solution was stirred for 1 hour
  2. customthe organic layer separated
  3. washwashed with water
  4. dry with materialdried (Na2SO4)
  5. customAfter drying the solvent
  6. customwas removed under vacuum

Sources & evidence

ORD record
ord-97998baa7601407f9326c5bd3f2974d5
Source dataset
uspto-grants-2007_06
Patent number
US07230121B2

Reaction notes

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