1T-0642 → HCID 58564023, compound

HRID 336202Notes

Reaction equation

HRID 336202 reaction equation
CC1(C)[O:7][C:6](=[O:8])[C:5]2([CH2:13][CH2:12][S:11](=[O:15])(=[O:14])[CH2:10][CH2:9]2)[C:4](=[O:16])[O:3]1>Cl>[O:14]=[S:11]1(=[O:15])[CH2:12][CH2:13][C:5]([C:4]([OH:16])=[O:3])([C:6]([OH:8])=[O:7])[CH2:9][CH2:10]1

Participants

3

Reactant 1

HCID 14917331T-0642

Product 1

HCID 58564023HCID 58564023, compound

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Procedure

3,3-Dimethyl-9,9-dioxo-2,4-dioxa-9λ6-thia-spiro[5.5]undecane-1,5-dione (200 mg; 0.763 mmol) is dispersed in 2M HCl aqueous solution (2 mL) and the vial is placed into microwave oven for 23 minutes at 100° C. After cooling, the reaction mixture is extracted with diethyl ether once. The aqueous layer is saturated with solid sodium chloride and extracted with 50% THF in ethyl acetate three times. The organics are combined and dried over Na2SO4, filtered and concentrated in vacuo to afford the title compound.

Workup

  1. temperatureAfter cooling
  2. extractionthe reaction mixture is extracted with diethyl ether once
  3. extractionextracted with 50% THF in ethyl acetate three times
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

Sources & evidence

ORD record
ord-a24b1d4bee274223adedeed75dbcc4e9
Source dataset
uspto-grants-2014_11
Patent number
US08889670B2

Reaction notes

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