HomeMCPWorkbenchSkills
HomeWorkbenchNotificationsMe
llms.txt · MCP GuidePrivacy Policy · Terms of Service · Supportv1.8.0
  1. Home
  2. /Reaction

Water → [2-(4-Bromo-phenyl)-2-(4-chloro-phenyl)ethyl]-methyl-amine

HRID 924726
Notes
Print preview

Reaction equation

HRID 924726 reaction equation
[Cl-:1].[Al+3].[Cl-].[Cl-].[Br:5][C:6]1[CH:11]=[CH:10][C:9]([CH:12](O)[CH2:13][NH:14][CH3:15])=[CH:8][CH:7]=1.O>ClC1C=CC=CC=1>[Br:5][C:6]1[CH:11]=[CH:10][C:9]([CH:12]([C:6]2[CH:11]=[CH:10][C:9]([Cl:1])=[CH:8][CH:7]=2)[CH2:13][NH:14][CH3:15])=[CH:8][CH:7]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 962WaterHCID 6451240Aluminum(III) ChlorideHCID 219434331-(4-Bromophenyl)-2-methylaminoethanol

Product 1

HCID 57691393[2-(4-Bromo-phenyl)-2-(4-chloro-phenyl)ethyl]-methyl-amine

Reagents, catalysts & solvents 1

HCID 7964ChlorobenzeneSolvent

Procedure

Aluminium chloride (278 mg, 2.087 mmol) was added portionwise to a stirred solution of 1-(4-Bromo-phenyl)-2-methylamino-ethanol (160 mg, 0.696 mmol) in chlorobenzene (3 ml) and the reaction mixture stirred at room temperature for 17 hours. Water (2 ml) was added dropwise and the reaction mixture was then partitioned between dichloromethane (100 ml) and saturated NaHCO3 (30 ml). The organic layer was dried (MgSO4), filtered and concentrated under reduced pressure. The crude product was then purified by Phenomenex_Strata_SCX column chromatography eluting with methanol followed by 2N ammonia in methanol to afford the desired product. LC/MS: (PS-B3) Rt 3.58 [M+H]+ 324.

Workup

  1. customthe reaction mixture was then partitioned between dichloromethane (100 ml) and saturated NaHCO3 (30 ml)
  2. dry with materialThe organic layer was dried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe crude product was then purified by Phenomenex_Strata_SCX column chromatography
  6. washeluting with methanol

Sources & evidence

ORD record
ord-b39ee0ce442b41e195503835c80ad7ae
Source dataset
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09283226B2

Reaction notes

Loading…

On this pageParticipantsProcedureWorkupSources & evidenceReaction notes