Methanol → HCID 68937866, compound

HRID 1723722Notes

Reaction equation

HRID 1723722 reaction equation
[OH-].[Na+].[I-].[OH:4][CH2:5][CH2:6][N+:7]1([CH3:24])[CH2:12][CH2:11][N:10]([C:13](=[O:23])[NH:14][C:15]2[CH:20]=[C:19]([Cl:21])[CH:18]=[C:17]([Cl:22])[CH:16]=2)[CH2:9][CH2:8]1.CO>O>[Cl-:21].[OH:4][CH2:5][CH2:6][N+:7]1([CH3:24])[CH2:12][CH2:11][N:10]([C:13](=[O:23])[NH:14][C:15]2[CH:20]=[C:19]([Cl:21])[CH:18]=[C:17]([Cl:22])[CH:16]=2)[CH2:9][CH2:8]1

Participants

5

Reactant 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 68935274HCID 68935274, compound

Product 1

HCID 68937866HCID 68937866, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

Amberlite IRA-400 resin (100 ml), a strongly basic ion exchange resin, was added with 1 N aqueous sodium hydroxide (200 ml), left for 30 minutes, then collected by filtration through a glass filter and washed with distilled water. Then, the resin was added with 1 N aqueous hydrochloric acid (200 ml), left for one hour, then collected by filtration through a glass filter and washed with distilled water until pH of the filtrate became neutral to obtain an ion exchanger. 1-(2-Hydroxyethyl)-1-methyl-4-(3,5-dichlorophenylcarbamoyl)piperazinium iodide obtained in Example 11 was subjected to ion exchange chromatography (methanol:water=10:1) using the resulting ion exchanger to obtain the title compound. Melting point: 154-156° C.

Workup

  1. filtrationcollected by filtration through a glass
  2. filtrationfilter
  3. washwashed with distilled water
  4. additionThen, the resin was added with 1 N aqueous hydrochloric acid (200 ml)
  5. waitleft for one hour
  6. filtrationcollected by filtration through a glass
  7. filtrationfilter
  8. washwashed with distilled water until pH of the filtrate
  9. customto obtain an ion exchanger

Sources & evidence

ORD record
ord-b57981a527124945ae03898160454773
Source dataset
uspto-grants-2009_02
Patent number
US07485646B2

Reaction notes

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