2-Methylpiperidine → 69548-60-3

HRID 2057381Notes

Reaction equation

HRID 2057381 reaction equation
Cl[CH2:2][CH2:3][C:4]([N:6]1[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[C:10](=[O:17])[NH:9][C:8]2[CH:18]=[CH:19][CH:20]=[N:21][C:7]1=2)=[O:5].[CH3:22][CH:23]1[CH2:28][CH2:27][CH2:26][CH2:25][NH:24]1>C(O)(C)C>[CH3:22][CH:23]1[CH2:28][CH2:27][CH2:26][CH2:25][N:24]1[CH2:2][CH2:3][C:4]([N:6]1[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[C:10](=[O:17])[NH:9][C:8]2[CH:18]=[CH:19][CH:20]=[N:21][C:7]1=2)=[O:5]

Participants

4

Reactant 2

HCID 79742-MethylpiperidineHCID 1381057111-(3-chloropropionyl)-5,11-dihydro-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one

Product 1

HCID 305310169548-60-3

Reagents, catalysts & solvents 1

HCID 3776IsopropanolSolvent

Procedure

16 gm of 11-(3-chloropropionyl)-5,11-dihydro-6H-pyrido [2,3-b]-[1,4]benzodiazepin-6-one were, after addition of 20 ml of 2-methylpiperidine, refluxed for 1 hour in 200 ml of isopropanol, and the reaction mixture was then evaporated in vacuo to dryness. The residue was admixed with water, the mixture was made alkaline by addition of ammonia and extracted with chloroform. The evaporation residue of the chloroform extract was purified on a silica gel column. The eluate was then evaporated in vacuo to dryness, and the residue was recrystallized from isopropanol.

Workup

  1. customthe reaction mixture was then evaporated in vacuo to dryness
  2. additionby addition of ammonia
  3. extractionextracted with chloroform
  4. extractionThe evaporation residue of the chloroform extract
  5. customwas purified on a silica gel column
  6. customThe eluate was then evaporated in vacuo to dryness
  7. customthe residue was recrystallized from isopropanol

Sources & evidence

ORD record
ord-026c80aaf00f4be9a396cab91d4c9763
Source dataset
uspto-grants-1980_07
Patent number
US04210648

Reaction notes

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