Water → 888697-77-6

HRID 1964593Notes

Reaction equation

HRID 1964593 reaction equation
[F:1][C:2]1[CH:3]=[C:4]([S:9](Cl)(=[O:11])=[O:10])[CH:5]=[CH:6][C:7]=1[F:8].Cl.CN.[CH2:16]([N:18](CC)CC)C.O>ClCCl>[F:1][C:2]1[CH:3]=[C:4]([S:9]([NH:18][CH3:16])(=[O:11])=[O:10])[CH:5]=[CH:6][C:7]=1[F:8]

Participants

6

Reactant 4

HCID 962WaterHCID 8471TriethylamineHCID 27369133,4-Difluorobenzene-1-sulfonyl chlorideHCID 6364545Methylamine hydrochloride

Product 1

HCID 8467985888697-77-6Yield 30%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

Commercially available 3,4-difluorophenylsulfonylchloride (117 μL, 0.87 mmol) was dissolved in dichloromethane (5 mL), and methylamine hydrochloride (49 mg, 0.73 mmol) and triethylamine (203 μL, 1.45 mmol) were added, followed by stirring at room temperature for 2 hours. To the reaction solution, water (15 mL) was added, extraction was carried out twice with dichloromethane (15 mL), and washing was carried out with saturated brine (15 mL), followed by drying over sodium sulfate. The solvent was distilled off under reduced pressure, followed by vacuum drying, to afford the desired compound (44.7 mg, yield 30%) as a colorless oil.

Workup

  1. extractionextraction
  2. washwashing
  3. dry with materialby drying over sodium sulfate
  4. distillationThe solvent was distilled off under reduced pressure
  5. customdrying

Sources & evidence

ORD record
ord-82d86fa2c9cc4f4897aab3ac305771ba
Source dataset
uspto-grants-2013_04
Patent number
US08415359B2

Reaction notes

Loading…