Water → HCID 66915771, compound

HRID 2356953Notes

Reaction equation

HRID 2356953 reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([NH:8][C:9](=[O:23])[C:10]2[CH:15]=[C:14]([N+:16]([O-])=O)[CH:13]=[CH:12][C:11]=2[NH:19][CH:20]([CH3:22])[CH3:21])[CH2:4][CH2:3]1.O>C(O)(=O)C.[Zn]>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([NH:8][C:9](=[O:23])[C:10]2[CH:15]=[C:14]([NH2:16])[CH:13]=[CH:12][C:11]=2[NH:19][CH:20]([CH3:21])[CH3:22])[CH2:6][CH2:7]1

Participants

5

Procedure

2.0 g (6.5 mmol) of N-(4-methylpiperazin-1-yl)-2-isopropylamino-5-nitrobenzamide were dissolved in 40 ml of glacier acetic acid and 6.8 g of zinc powder were added gradually at 45-50° C. For workup, 40 ml of water were added, the mixture was extracted once with ethyl acetate, the water phase was alkalized with NaOH, and the mixture was extracted repeatedly with methylene chloride. The residue remaining after drying and concentration (1.9 g) could be used for the next reaction without further purification.

Workup

  1. extractionthe mixture was extracted once with ethyl acetate
  2. extractionthe mixture was extracted repeatedly with methylene chloride
  3. customafter drying
  4. concentrationconcentration (1.9 g)
  5. customcould be used for the next reaction without further purification

Sources & evidence

ORD record
ord-4f19a17c221c4ab4bcd084e3e3044679
Source dataset
uspto-grants-2010_07
Patent number
US07759379B2

Reaction notes

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