Chlorodifluoromethane → HCID 67422546, compound

HRID 629581Notes

Reaction equation

HRID 629581 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-92ee30b4603b4b719afa943273c85177
Source dataset
uspto-grants-2016_04
Patent number
US09315488B2

Reaction notes

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