Triethylamine → HCID 19068742, compound

HRID 1957242Notes

Reaction equation

HRID 1957242 reaction equation
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[NH2:6][C:7]1[CH:8]=[C:9]([C:14]2[C:19]([Cl:20])=[CH:18][C:17]([C:21]([F:24])([F:23])[F:22])=[CH:16][N:15]=2)[CH:10]=[CH:11][C:12]=1[Cl:13].C(N(CC)CC)C>C(Cl)Cl>[Cl:20][C:19]1[C:14]([C:9]2[CH:10]=[CH:11][C:12]([Cl:13])=[C:7]([N:6]([S:2]([CH3:1])(=[O:4])=[O:3])[S:2]([CH3:1])(=[O:4])=[O:3])[CH:8]=2)=[N:15][CH:16]=[C:17]([C:21]([F:24])([F:23])[F:22])[CH:18]=1

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 15766880HCID 15766880, compound

Product 1

HCID 19068742HCID 19068742, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

2.4 g (21.0 mmol) of methanesulfonyl chloride were slowly added dropwise to a mixture of 3.0 g (9.77 mmol) of 2-(3-amino-4-chlorophenyl)-3-chloro-5-trifluoromethylpyridine, 2.2 g (22.4 mmol) of triethylamine and 50 ml of anhydrous methylene chloride at 0°-5° C. The mixture was stirred at 20°-25° C. for about 15 hours and then washed twice with water, dried over sodium sulfate and finally concentrated. The residue was stirred with ether, filtered off with suction and dried under reduced pressure. Yield: 3.6 g (87%) of colorless crystals of melting point 230°-231° C.

Workup

  1. washwashed twice with water
  2. dry with materialdried over sodium sulfate
  3. concentrationfinally concentrated
  4. stirringThe residue was stirred with ether
  5. filtrationfiltered off with suction
  6. customdried under reduced pressure

Sources & evidence

ORD record
ord-8741899b6252463b9f91bc655a1d8a8f
Source dataset
uspto-grants-1998_07
Patent number
US05783522

Reaction notes

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