Sodium Bicarbonate → HCID 57126064, compound

HRID 1590587Notes

Reaction equation

HRID 1590587 reaction equation
C(=O)(O)[O-].[Na+].[CH2:6]([N:8]([CH2:32][CH3:33])[C:9]1[CH:14]=[CH:13][C:12]([S:15]([N:18]2[CH2:22][CH:21]([O:23][Si](C(C)(C)C)(C)C)[CH2:20][C:19]2=[S:31])(=[O:17])=[O:16])=[CH:11][CH:10]=1)[CH3:7]>C(Cl)Cl>[CH2:32]([N:8]([CH2:6][CH3:7])[C:9]1[CH:14]=[CH:13][C:12]([S:15]([N:18]2[CH2:22][CH:21]([OH:23])[CH2:20][C:19]2=[S:31])(=[O:16])=[O:17])=[CH:11][CH:10]=1)[CH3:33]

Participants

4

Reactant 2

HCID 516892Sodium BicarbonateHCID 57157513HCID 57157513, compound

Product 1

HCID 57126064HCID 57126064, compoundYield 72.6%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

30 cm3 of sodium bicarbonate is added at -20° C. over one hour to a solution of 1.3 g of 1-[[4-(diethylamino)-phenyl]-sulphonyl]-4-[(1,1-dimethylethyl)-dimethylsilyloxy]-2-pyrrolidine thione obtained above, in 30 cm3 of methylene chloride. The mixture is agitated for 16 hours at ambient temperature, decanted, extracted with methylene chloride, the extracts are dried and evaporated to dryness. After crystallization from a chloroform - hexane mixture, 700 mg of the desired product is obtained. M.p=149-150° C.

Workup

  1. customdecanted
  2. extractionextracted with methylene chloride
  3. customthe extracts are dried
  4. customevaporated to dryness
  5. customAfter crystallization from a chloroform - hexane mixture

Sources & evidence

ORD record
ord-ea649164401b4bd0a98b4f323d97e7bb
Source dataset
uspto-grants-1993_04
Patent number
US05204341

Reaction notes

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