Sodium Carbonate → HCID 54436504, compound

HRID 1416991Notes

Reaction equation

HRID 1416991 reaction equation
[Cl:1][CH2:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][S:10]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[O:11])=[CH:5][CH:4]=1.ClC1C=CC=C(C(OO)=[O:26])C=1.C([O-])(O)=O.[Na+].C([O-])([O-])=O.[Na+].[Na+]>C(Cl)Cl.O>[Cl:1][CH2:2][C:3]1[CH:4]=[CH:5][C:6]([CH2:9][S:10]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)(=[O:26])=[O:11])=[CH:7][CH:8]=1

Participants

7

Reactant 4

HCID 10340Sodium CarbonateHCID 70297m-Chloroperbenzoic acidHCID 516892Sodium BicarbonateHCID 10967404HCID 10967404, compound2×

Product 1

HCID 54436504HCID 54436504, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 6344DichloromethaneSolvent2×

Procedure

27.61 g (0.104 mol) (1a) was dissolved in 400 ml CH2Cl2. This solution was added dropwise to an ice-cooled solution of 36.03 g (0.208 mol) 3-chloroperbenzoic acid in 600 ml CH2Cl2 and 33.61 g (0.375 mol) NaHCO3 in 200 ml H2O. After the addition of (1a) the mixture was allowed to warm up to room temperature, and this was followed by another 2 hours' stirring. The reaction mixture was then poured into 500 ml 5% Na2CO3 solution. The organic layer was washed with 500 ml 5% Na2S2O3 solution. The CH2Cl2 was dried over MgSO4 and evaporated. The precipitate was purified by recrystallization from hexane/toluene. Yield: 26.65 g (91%); m.p.=170.3-170.9° C. (dec.)

Workup

  1. washThe organic layer was washed with 500 ml 5% Na2S2O3 solution
  2. dry with materialThe CH2Cl2 was dried over MgSO4
  3. customevaporated
  4. customThe precipitate was purified by recrystallization from hexane/toluene

Sources & evidence

ORD record
ord-896a9e74c1e2492f9fb2a173f26d6132
Source dataset
uspto-grants-1999_06
Patent number
US05917003

Reaction notes

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