Potassium Iodide → HCID 20360377, compound

HRID 2082678Notes

Reaction equation

HRID 2082678 reaction equation
Cl.Cl[CH2:3][CH2:4][NH:5][CH:6]([C:14]1[CH:19]=[CH:18][C:17]([F:20])=[CH:16][CH:15]=1)[C:7]1[CH:12]=[CH:11][C:10]([F:13])=[CH:9][CH:8]=1.[F:21][C:22]1[CH:27]=[CH:26][C:25]([N:28]2[C:32]3([CH2:37][CH2:36][NH:35][CH2:34][CH2:33]3)[C:31](=[O:38])[NH:30][CH2:29]2)=[CH:24][CH:23]=1.C(=O)([O-])[O-].[Na+].[Na+].[I-].[K+]>O.CC(C)CC(=O)C>[F:13][C:10]1[CH:11]=[CH:12][C:7]([CH:6]([NH:5][CH2:4][CH2:3][N:35]2[CH2:34][CH2:33][C:32]3([N:28]([C:25]4[CH:24]=[CH:23][C:22]([F:21])=[CH:27][CH:26]=4)[CH2:29][NH:30][C:31]3=[O:38])[CH2:37][CH2:36]2)[C:14]2[CH:19]=[CH:18][C:17]([F:20])=[CH:16][CH:15]=2)=[CH:8][CH:9]=1

Participants

7

Reactant 4

HCID 4875Potassium IodideHCID 10340Sodium CarbonateHCID 939151-(4-Fluorophenyl)-1,3,8-triazaspiro(4.5)decan-4-oneHCID 3017749N-[Bis(4-fluorophenyl)methyl]-2-chloroethan-1-amine--hydrogen chloride (1/1)

Product 1

HCID 20360377HCID 20360377, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 7909Methyl Isobutyl KetoneSolvent

Procedure

A mixture of 8 parts of N-(2-chloroethyl)-4-fluoro-α-(4-fluorophenyl)benzenemethanamine hydrochloride, 5.7 parts of 1-(4-fluorophenyl)-1,3,8-triazaspiro[4,5]decan-4-one, 10 parts of sodium carbonate, 0.1 parts of potassium iodide and 80 parts of 4-methyl-2-pentanone is stirred and refluxed overnight. The reaction mixture is taken up in water and after stirring for a while, the precipitated product is filtered off. The product is washed with 4-methyl-2-pentanone, dried and crystallized from 4-methyl-2-pentanone (activated charcoal). It is filtered off and dried, yielding 4 parts of 8-[2-{[bis(4-fluorophenyl)methyl]amino}ethyl]-1-(4-fluorophenyl)-1,3,8-triazaspiro[4,5]decan-4-one; mp. 193° C.

Workup

  1. temperaturerefluxed overnight
  2. stirringafter stirring for a while
  3. filtrationthe precipitated product is filtered off
  4. washThe product is washed with 4-methyl-2-pentanone
  5. customdried
  6. customcrystallized from 4-methyl-2-pentanone (activated charcoal)
  7. filtrationIt is filtered off
  8. customdried

Sources & evidence

ORD record
ord-e57139be2a0b40d883432f90d9007e3a
Source dataset
uspto-grants-1978_04
Patent number
US04082755

Reaction notes

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