1-(2-Hydroxyethyl)piperazine → HCID 21525528, compound

HRID 1658767Notes

Reaction equation

HRID 1658767 reaction equation
Cl[CH2:2][C:3]([N:5]1[C:11]2[CH:12]=[C:13]([Br:17])[C:14]([Br:16])=[CH:15][C:10]=2[NH:9][C:8](=[O:18])[C:7]2[CH:19]=[CH:20][CH:21]=[N:22][C:6]1=2)=[O:4].[OH:23][CH2:24][CH2:25][N:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1>C(O)C>[Br:16][C:14]1[C:13]([Br:17])=[CH:12][C:11]2[N:5]([C:3](=[O:4])[CH2:2][N:29]3[CH2:30][CH2:31][N:26]([CH2:25][CH2:24][OH:23])[CH2:27][CH2:28]3)[C:6]3[N:22]=[CH:21][CH:20]=[CH:19][C:7]=3[C:8](=[O:18])[NH:9][C:10]=2[CH:15]=1

Participants

4

Reactant 2

HCID 76771-(2-Hydroxyethyl)piperazineHCID 21525527HCID 21525527, compound

Product 1

HCID 21525528HCID 21525528, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

11-Chloroacetyl-8,9-dibromo-6,11-dihydro-5H-pyrido[2,3-b][1,5]benzodiazepin-5-one (0.05 mole) and 0.13 mole 4-(2-hydroxyethyl)piperazine, dissolved in 800 ml. ethanol are heated to reflux for a period of 20 hours. The hot solution is then filtered, the filtrate evaporated in vacuo and the remaining residue recrystallized from 2-propanol to give 8,9-dibromo-6,11-dihydro-11-[[4-(2- hydroxyethyl)piperazino]acetyl]-5H-pyrido[2,3-b][1,5]-benzodiazepin-5-one.

Workup

  1. temperatureto reflux for a period of 20 hours
  2. filtrationThe hot solution is then filtered
  3. customthe filtrate evaporated in vacuo
  4. customthe remaining residue recrystallized from 2-propanol

Sources & evidence

ORD record
ord-4b075e21a3644d4f92c4dbba253d6a87
Source dataset
uspto-grants-1976_06
Patent number
US03966736

Reaction notes

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