Water → HCID 54297194, compound

HRID 848834Notes

Reaction equation

HRID 848834 reaction equation
Cl[C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:17])[C:9]2[CH:14]=[CH:13][C:12]([CH3:15])=[C:11]([CH3:16])[CH:10]=2)=[CH:4][CH:3]=1.[SH:18][CH2:19][CH2:20][OH:21].C([O-])([O-])=O.[K+].[K+].O>CC(N(C)C)=O.CCOCC>[OH:21][CH2:20][CH2:19][S:18][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:17])[C:9]2[CH:14]=[CH:13][C:12]([CH3:15])=[C:11]([CH3:16])[CH:10]=2)=[CH:4][CH:3]=1

Participants

7

Reactant 4

HCID 962WaterHCID 15672-MercaptoethanolHCID 11430Potassium CarbonateHCID 27574824-Chloro-3',4'-dimethylbenzophenone

Product 1

HCID 54297194HCID 54297194, compound

Reagents, catalysts & solvents 2

HCID 3283Diethyl EtherSolventHCID 31374DimethylacetamideSolvent

Procedure

12.2 g (0.05 mol) of 4'-chloro-3,4-dimethylbenzophenone and 4.3 g (0.055 mol) of 2-mercaptoethanol in 50 ml of dimethylacetamide are warmed to 95° under nitrogen. 13.8 g (0.1 mol) of calcined K2CO3 are then added. The suspension is kept at 90°-100° C. for 6 hours. 100 ml of water are poured over the resulting reaction mixture and the product is taken up in ether. The ether layer is washed with water, dried over Na2SO4 and concentrated. The resulting crystals are recrystallised from methanol and dried in vacuo at 60° C. Yield: 10.1 g (71%). Melting point 92-93° C.

Workup

  1. washThe ether layer is washed with water
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated
  4. customThe resulting crystals are recrystallised from methanol
  5. customdried in vacuo at 60° C

Sources & evidence

ORD record
ord-33aed8b0096f46d98f32f82f518b8b47
Source dataset
uspto-grants-1981_10
Patent number
US04297513

Reaction notes

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