Diethyl Ether → HCID 131731751, compound

HRID 2403528Notes

Reaction equation

HRID 2403528 reaction equation
[F:1][C:2]([C:5]1[CH:6]=[C:7]([CH:9]=[CH:10][CH:11]=1)[NH2:8])([F:4])[CH3:3].[Cl:12][CH2:13][CH2:14][NH:15][CH2:16][CH2:17]Cl.C(OCC)C>ClC1C=CC=CC=1>[ClH:12].[F:1][C:2]([C:5]1[CH:6]=[C:7]([N:8]2[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)[CH:9]=[CH:10][CH:11]=1)([F:4])[CH3:3]

Participants

5

Reactant 3

HCID 3283Diethyl EtherHCID 9533Bis(2-chloroethyl)amineHCID 234450923-(1,1-Difluoroethyl)aniline

Product 1

HCID 131731751HCID 131731751, compoundYield 91%

Reagents, catalysts & solvents 1

HCID 7964ChlorobenzeneSolvent

Procedure

A mixture of 2.5 g (15.9 mmol) of 3-(1,1-difluoroethyl)aniline and 2.8 g (15.9 mmol) of bis(2-chloroethyl)amine in 20 mL of chlorobenzene is refluxed overnight. After cooling to room temperature, diethyl ether is added and precipitation occurs. The solid is filtered, washed with diethyl ether and dried under reduced pressure to give 3.8 g (90%) of 1-[3-(1,1-difluoro-ethyl)phenyl]piperazine, hydrochloride as a white solid.

Workup

  1. temperatureis refluxed overnight
  2. customprecipitation
  3. filtrationThe solid is filtered
  4. washwashed with diethyl ether
  5. customdried under reduced pressure

Sources & evidence

ORD record
ord-4ec0d0a106cd47ac8f125d653248e49c
Source dataset
uspto-grants-2014_08
Patent number
US08802678B2

Reaction notes

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