1-Methylpiperazine → HCID 20515521, compound

HRID 1902475Notes

Reaction equation

HRID 1902475 reaction equation
Cl[CH2:2][C:3]([N:5]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[NH:9][C:8](=[O:16])[C:7]2[N:17]([CH3:22])[C:18]([CH3:21])=[C:19]([CH3:20])[C:6]1=2)=[O:4].[CH3:23][N:24]1[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]1.C(=O)(O)[O-].[Na+]>O1CCOCC1>[CH3:22][N:17]1[C:7]2[C:8](=[O:16])[NH:9][C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=3[N:5]([C:3](=[O:4])[CH2:2][N:27]3[CH2:28][CH2:29][N:24]([CH3:23])[CH2:25][CH2:26]3)[C:6]=2[C:19]([CH3:20])=[C:18]1[CH3:21]

Participants

5

Reactant 3

HCID 531671-MethylpiperazineHCID 516892Sodium BicarbonateHCID 20515513HCID 20515513, compound

Product 1

HCID 20515521HCID 20515521, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

289 g of 4-chloroacetyl-1,2,3-trimethyl-1,4,9,10-tetrahydropyrrolo[3,2-b][1,5]benzodiazepin-10-one, 200 mg of N-methylpiperazine and 10 ml of dry dioxane are warmed at 70° to 80° C. for 2.5 hours. 10 ml of saturated aqueous sodium bicarbonate solution are added thereto, and the resulting mixture is extracted several times with ethyl acetate. The combined extracts are dried over sodium sulfate and concentrated in vacuo. The resulting oil is taken up in a little dioxane/acetonitrile and is brought to crystallization.

Workup

  1. extractionthe resulting mixture is extracted several times with ethyl acetate
  2. dry with materialThe combined extracts are dried over sodium sulfate
  3. concentrationconcentrated in vacuo
  4. customis brought to crystallization

Sources & evidence

ORD record
ord-800513c5a97d44e2b0e275601b9b45e7
Source dataset
uspto-grants-1982_12
Patent number
US04363816

Reaction notes

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