Chloroform → HCID 84762869, compound

HRID 1991487Notes

Reaction equation

HRID 1991487 reaction equation
Cl.[F:2][C:3]1([F:10])[CH2:8][CH2:7][CH:6]([NH2:9])[CH2:5][CH2:4]1.[OH-].[Na+].[CH:13](Cl)(Cl)Cl.C(Cl)Cl>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.O>[F:2][C:3]1([F:10])[CH2:8][CH2:7][CH:6]([N+:9]#[C-:13])[CH2:5][CH2:4]1

Participants

7

Reactant 4

HCID 6212ChloroformHCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 231506694,4-Difluorocyclohexan-1-amine hydrochloride

Product 1

HCID 84762869HCID 84762869, compound

Reagents, catalysts & solvents 2

HCID 94433Tetrabutylammonium hydrogen sulfateCatalystHCID 962WaterSolvent

Procedure

4,4-Difluoro-cyclohexylamine hydrochloride (1.0 g, 5.8 mmol, 1 equiv.) was added to a mixture of NaOH (1.5 g, 37 mmol, 6.3 equiv.) and tetrabutylammonium hydrogen sulfate (40 mg, 0.12 mmol, 0.02 equiv.) in water (2.5 ml), chloroform (3 ml, 37 mmol) 6.3 equiv.) and DCM (5 ml). The mixture was stirred at room temperature for 72 h and the crude extracted with DCM. The product was isolated via Kieslgel chromatography.

Workup

  1. extractionthe crude extracted with DCM
  2. customThe product was isolated via Kieslgel chromatography

Sources & evidence

ORD record
ord-3c36635ab26346a2bf15c52901ebd981
Source dataset
uspto-grants-2010_01
Patent number
US07645785B2

Reaction notes

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