Chlorodifluoromethane → HCID 67422546, compound

HRID 2044996Notes

Reaction equation

HRID 2044996 reaction equation
[OH-].[Na+].COCCOCCN(CCOCCOC)CCOCCOC.[F:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=1[SH:32].Cl[CH:34]([F:36])[F:35]>C1C=CC=CC=1>[F:35][CH:34]([S:32][C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][C:26]=1[F:25])[F:36]

Participants

6

Reactant 4

HCID 6372ChlorodifluoromethaneHCID 14798Sodium HydroxideHCID 112414Ethanamine, 2-(2-methoxyethoxy)-N,N-bis[2-(2-methoxyethoxy)ethyl]-HCID 5202162-Fluorothiophenol

Product 1

HCID 67422546HCID 67422546, compound

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent

Conditions

Temperature
80 °C

Procedure

Powdered NaOH (31.2 g), tris(2-(2-methoxyethoxy)ethyl)amine (5 mL) and 2-fluorobenzene thiol (33.6 mL) in benzene (400 mL) was saturated with chlorodifluoromethane, stirred at 80° C. for 30 minutes and filtered through diatomaceous earth (Celite®). The filtrate was washed with saturated NaHCO3 and the water layer was extracted with diethyl ether. The extracts were combined and dried (MgSO4), filtered and concentrated.

Workup

  1. filtrationfiltered through diatomaceous earth (Celite®)
  2. washThe filtrate was washed with saturated NaHCO3
  3. extractionthe water layer was extracted with diethyl ether
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated

Sources & evidence

ORD record
ord-1096818e16f24db2b15c2a3f95b7d916
Source dataset
uspto-grants-2013_11
Patent number
US08586754B2

Reaction notes

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