Calcium Hydroxide → HCID 13013925, compound

HRID 444139Notes

Reaction equation

HRID 444139 reaction equation
[O:1]=[C:2]1[C:8]2[CH:9]=[CH:10][C:11]([C:13]([O:15][CH3:16])=[O:14])=[CH:12][C:7]=2[S:6][C:5]2[CH:17]=[CH:18][CH:19]=[CH:20][C:4]=2[NH:3]1.[OH-:21].[Ca+2].[OH-:23]>ClC1C=CC=C(C(OO)=O)C=1.C(Cl)(Cl)Cl>[O:1]=[C:2]1[C:8]2[CH:9]=[CH:10][C:11]([C:13]([O:15][CH3:16])=[O:14])=[CH:12][C:7]=2[S:6](=[O:23])(=[O:21])[C:5]2[CH:17]=[CH:18][CH:19]=[CH:20][C:4]=2[NH:3]1

Participants

5

Reactant 2

HCID 6093208Calcium HydroxideHCID 13013924HCID 13013924, compound

Product 1

HCID 13013925HCID 13013925, compound

Reagents, catalysts & solvents 2

HCID 6212ChloroformSolventHCID 70297m-Chloroperbenzoic acidSolvent

Procedure

Dissolve 570 mg (2 mmoles) of the ester of Example 2 in a mixture of 2.3 gm of m-chloroperbenzoic acid and 75 cc of chloroform and stir for 12 hours at room temperature. Basify with calcium hydroxide. Filter and evaporate to dryness. Chromatograph the residue over silica gel eluding with 30% ethyl acetate in benzene. Collect the sulfone fractions and evaporate to dryness. Stir the residue in ether for 30 minutes, filter and dry to obtain the title product (m.p. 300°-302° C.), sintered around 295° C.).

Workup

  1. filtrationFilter
  2. customevaporate to dryness
  3. customCollect the sulfone fractions
  4. customevaporate to dryness
  5. stirringStir the residue in ether for 30 minutes
  6. filtrationfilter
  7. customdry

Sources & evidence

ORD record
ord-b74a83e591f24b1b9cae8e4709f34129
Source dataset
uspto-grants-1981_04
Patent number
US04263207

Reaction notes

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