Potassium Hydroxide → HCID 86707267, compound

HRID 576048Notes

Reaction equation

HRID 576048 reaction equation
[OH-].[K+].[F:3][C:4]1[CH:9]=[CH:8][C:7]([NH:10][S:11]([C:14]2[CH:15]=[C:16]3[C:21](=[CH:22][CH:23]=2)[CH2:20][N:19](C(=O)C(F)(F)F)[CH2:18][CH2:17]3)(=[O:13])=[O:12])=[CH:6][CH:5]=1>C(O)C>[F:3][C:4]1[CH:5]=[CH:6][C:7]([NH:10][S:11]([C:14]2[CH:15]=[C:16]3[C:21](=[CH:22][CH:23]=2)[CH2:20][NH:19][CH2:18][CH2:17]3)(=[O:13])=[O:12])=[CH:8][CH:9]=1

Participants

4

Reactant 2

HCID 14797Potassium HydroxideHCID 86707268HCID 86707268, compound

Product 1

HCID 86707267HCID 86707267, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

An aqueous solution (10 mL) of potassium hydroxide (2.24 g, 40.0 mmol) was added to a suspension of N-(4-fluorophenyl)-2-(trifluoroacetyl)-1,2,3,4-tetrahydroisoquinoline-6-sulfonamide obtained (8.05 g, 20.0 mmol) in ethanol (40 mL), and the mixture was stirred at room temperature for 15 hr. The mixture was concentrated under reduced presesure and then diluted with water. While cooling in ice, 3 mol/L hydrochloric acid was added dropwise thereto to adjust the pH to 7 to 8. A precipitated solid was collected by filtration to afford the title compound as a colorless powder (6.04 g).

Workup

  1. concentrationThe mixture was concentrated under reduced presesure
  2. additiondiluted with water
  3. temperatureWhile cooling in ice
  4. addition3 mol/L hydrochloric acid was added dropwise
  5. filtrationA precipitated solid was collected by filtration

Sources & evidence

ORD record
ord-7562a16e98154e6b8e8c7ff35c912276
Source dataset
uspto-grants-2015_05
Patent number
US09035059B2

Reaction notes

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