Toluene → HCID 23459029, compound

HRID 1680074Notes

Reaction equation

HRID 1680074 reaction equation
Cl[CH2:2][CH2:3][O:4][C:5]([O:20][CH2:21][CH2:22]Cl)([C:12]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)=[O:13])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[CH3:24][N:25]1[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]1.[C:31]1([CH3:37])C=CC=CC=1>O>[CH3:24][N:25]1[CH2:30][CH2:29][N:28]([CH2:2][CH2:3][O:4][C:5]([O:20][CH2:21][CH2:22][N:28]2[CH2:37][CH2:31][N:25]([CH3:24])[CH2:26][CH2:27]2)([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=2)[C:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[O:13])[CH2:27][CH2:26]1

Participants

5

Reactant 3

HCID 1140TolueneHCID 531671-MethylpiperazineHCID 14762563HCID 14762563, compound

Product 1

HCID 23459029HCID 23459029, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

With stirring, 23.6 g (0.067 mole) of benzil-di-(2-chloroethyl)ketal and 120 g (1.2 moles) of N-methylpiperazine are kept for 3 hours at 95° C. After cooling, 250 ml of toluene are added and the reaction mixture is poured into water. The aqueous layer is extracted with toluene and the toluene layer is subsequently washed neutral with water. The toluene layer is dried over Na2SO4, concentrated and dried in a high vacuum.

Workup

  1. temperatureAfter cooling
  2. extractionThe aqueous layer is extracted with toluene
  3. dry with materialThe toluene layer is dried over Na2SO4
  4. concentrationconcentrated
  5. customdried in a high vacuum

Sources & evidence

ORD record
ord-ccc47fcc27b045ca8c37118ff53dade8
Source dataset
uspto-grants-1981_06
Patent number
US04271294

Reaction notes

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