Ammonia → HCID 54502175, compound

HRID 2290479Notes

Reaction equation

HRID 2290479 reaction equation
Cl.Cl.[Cl:3][C:4]1[CH:27]=[CH:26][CH:25]=[CH:24][C:5]=1[CH2:6][N:7]1[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][C:15]2[CH:23]=[CH:22][C:18]([C:19](Cl)=[O:20])=[CH:17][CH:16]=2)[CH2:9][CH2:8]1.O1CCOCC1.[NH3:34]>O>[Cl:3][C:4]1[CH:27]=[CH:26][CH:25]=[CH:24][C:5]=1[CH2:6][N:7]1[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][C:15]2[CH:23]=[CH:22][C:18]([C:19]([NH2:34])=[O:20])=[CH:17][CH:16]=2)[CH2:9][CH2:8]1

Participants

5

Reactant 3

HCID 222AmmoniaHCID 312751,4-Dioxane2×HCID 20232452HCID 20232452, compound

Product 1

HCID 54502175HCID 54502175, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

To a solution of 14.2 g. (31.5 mmole) 4-{2-[1-(2-chlorobenzyl)-piperazin-4-yl]-ethyl}-benzoyl chloride dihydrochloride and 150 ml. dioxan, there is added dropwise, while stirring at ambient temperature, within the course of 30 minutes, a solution of 100 ml. concentrated aqueous ammonia in 50 ml. dioxan. The reaction mixture is stirred for a further 30 minutes and then sufficient water is added thereto to precipitate out the desired amide. After suction filtration, drying and recrystallisation from toluene, there are obtained 8.5 g. (75% of theory) of amide; m.p. 170°-173° C.

Workup

  1. stirringThe reaction mixture is stirred for a further 30 minutes
  2. customto precipitate out the desired amide
  3. filtrationAfter suction filtration
  4. customdrying
  5. customrecrystallisation from toluene, there
  6. customare obtained 8.5 g

Sources & evidence

ORD record
ord-cea76fd9df9c4f02baa3e57bc95b86d9
Source dataset
uspto-grants-1986_10
Patent number
US04616086

Reaction notes

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