Hydrochloric Acid → HCID 117704078, compound

HRID 1049877Notes

Reaction equation

HRID 1049877 reaction equation
C([NH:4][C:5]1[S:6][C:7]([S:13]([C:16]2[CH:21]=[CH:20][C:19]([O:22][C:23]([F:26])([F:25])[F:24])=[CH:18][CH:17]=2)(=[O:15])=[O:14])=[CH:8][C:9]=1[C:10]([NH2:12])=[O:11])(=O)C.Cl>O1CCOCC1>[NH2:4][C:5]1[S:6][C:7]([S:13]([C:16]2[CH:17]=[CH:18][C:19]([O:22][C:23]([F:26])([F:24])[F:25])=[CH:20][CH:21]=2)(=[O:14])=[O:15])=[CH:8][C:9]=1[C:10]([NH2:12])=[O:11]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 117703988HCID 117703988, compound

Product 1

HCID 117704078HCID 117704078, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Conditions

Temperature
105 °C

Procedure

The 2-acetylamino-5-(4-trifluoromethoxy-benzenesulfonyl)-thiophene-3-carboxylic acid amide (10 g, crude) is dissolved in 1,4-dioxane (300 mL) and an aqueous solution of 2 M HCl (100 mL). This mixture is stirred at 105° C. overnight, after which the dioxane is concentrated in vacuo and the remaining aqueous basified with an aqueous solution of 5 M NaOH to pH-8-9. The resulting precipitate is collected by filtration, washed thoroughly with water and dried to afford the desired compound.

Workup

  1. concentrationafter which the dioxane is concentrated in vacuo
  2. filtrationThe resulting precipitate is collected by filtration
  3. washwashed thoroughly with water
  4. customdried

Sources & evidence

ORD record
ord-815c8b6d939b458cb8d35d9f0697f45f
Source dataset
uspto-grants-2016_07
Patent number
US09382254B2

Reaction notes

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