Trichloromethanesulfenyl chloride → HCID 18788458, compound

HRID 1106471Notes

Reaction equation

HRID 1106471 reaction equation
[Cl:1][C:2](Cl)(Cl)[S:3]Cl.[CH3:7][C:8]1[CH:16]=[C:15]([CH3:17])[CH:14]=[C:13]([CH3:18])[C:9]=1[C:10]([NH2:12])=[NH:11].[OH-].[Na+]>ClCCl.O>[Cl:1][C:2]1[S:3][N:12]=[C:10]([C:9]2[C:8]([CH3:7])=[CH:16][C:15]([CH3:17])=[CH:14][C:13]=2[CH3:18])[N:11]=1

Participants

6

Reactant 3

HCID 11666Trichloromethanesulfenyl chlorideHCID 14798Sodium HydroxideHCID 18788461Mesitylformamidin

Product 1

HCID 18788458HCID 18788458, compoundYield 99.1%

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 6344DichloromethaneSolvent

Procedure

2.2 g of trichloromethanesulfenyl chloride are introduced into a solution of 2 g of 2,4,6-trimethyl benzamidine in 16 ml of dichloromethane under an inert atmosphere at about -20° C., followed by the slow addition of 2 g of NaOH dissolved in 3.2 ml of water at about -10° C. After 1 hour at about -5° C., the precipitate formed is isolated and the organic phase is separated and washed with 6 ml of water. After being dried over K2CO3, it is concentrated under reduced pressure to give 2.8 g of the desired product in the form of an oil, which may be used without purification.

Workup

  1. customthe precipitate formed
  2. customis isolated
  3. customthe organic phase is separated
  4. washwashed with 6 ml of water
  5. dry with materialAfter being dried over K2CO3, it
  6. concentrationis concentrated under reduced pressure

Sources & evidence

ORD record
ord-a5b6cabd4efd497793249aaeb8c6a284
Source dataset
uspto-grants-2000_05
Patent number
US06057318

Reaction notes

Loading…