Water → HCID 67126688, compound

HRID 2168440Notes

Reaction equation

HRID 2168440 reaction equation
[Cl:1][C:2]1[CH:3]=[C:4]([S:21]([NH2:24])(=[O:23])=[O:22])[CH:5]=[N:6][C:7]=1[O:8][CH2:9][C:10]1([F:20])[CH2:19][CH2:18][C:13]2(OCC[O:14]2)[CH2:12][CH2:11]1.C1(C)C=CC(S([O-])(=O)=O)=CC=1.[NH+]1C=CC=CC=1.O>CC(C)=O.ClCCl>[Cl:1][C:2]1[CH:3]=[C:4]([S:21]([NH2:24])(=[O:23])=[O:22])[CH:5]=[N:6][C:7]=1[O:8][CH2:9][C:10]1([F:20])[CH2:19][CH2:18][C:13](=[O:14])[CH2:12][CH2:11]1

Participants

6

Reactant 3

HCID 962WaterHCID 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)HCID 672259855-Chloro-6-((8-fluoro-1,4-dioxaspiro[4.5]decan-8-yl)methoxy)pyridine-3-sulfonamide

Product 1

HCID 67126688HCID 67126688, compound

Reagents, catalysts & solvents 2

HCID 180AcetoneSolventHCID 6344DichloromethaneSolvent

Conditions

Temperature
100 °C

Procedure

To a solution of EXAMPLE 512C (1.6 g) and pyridinium p-toluenesulfonate (1.2 g) in acetone (10 mL) was added water (2 mL) and the mixture was stirred in a CEM Discover microwave reactor at 100° C. for 10 minutes. The mixture was diluted with dichloromethane (300 mL) and washed with aqueous NaHCO3, water, brine and dried over Na2SO4. Filtration and evaporation of the solvent gave the crude product.

Workup

  1. washwashed with aqueous NaHCO3, water, brine
  2. dry with materialdried over Na2SO4
  3. filtrationFiltration and evaporation of the solvent

Sources & evidence

ORD record
ord-3439c801214144e6ae80bf94b57f78dc
Source dataset
uspto-grants-2015_06
Patent number
US09045420B2

Reaction notes

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