Propylamine → HCID 178456819, compound

HRID 1078544Notes

Reaction equation

HRID 1078544 reaction equation
Cl[C:2]1[C:3]2[CH:18]=[CH:17][CH:16]=[N:15][C:4]=2[N:5]([CH2:13][CH3:14])[C:6]2[N:12]=[CH:11][CH:10]=[CH:9][C:7]=2[N:8]=1.[CH2:19]([NH2:22])[CH2:20][CH3:21]>C1(C)C=CC=CC=1>[CH2:13]([N:5]1[C:4]2[N:15]=[CH:16][CH:17]=[CH:18][C:3]=2[C:2]([NH:22][CH2:19][CH2:20][CH3:21])=[N:8][C:7]2[CH:9]=[CH:10][CH:11]=[N:12][C:6]1=2)[CH3:14]

Participants

4

Reactant 2

HCID 7852Propylamine2×HCID 19427676HCID 19427676, compound

Product 1

HCID 178456819HCID 178456819, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

A mixture of 6-chloro-11-ethyl-11H-dipyrido[3,2-b:2',3'-e][1,4]diazepine (0.7 g, n-propylamine (0.8 g), and toluene (25 mL) was heated at reflux for ten days. At two day intervals during the ten day period, additional 1.6 g portions of n-propylamine was added to the refluxing mixture. The mixture was then concentrated in vacuo and the residue chromatographed over silica gel (eluted with 20% ethyl acetate/hexane) to give 0.15 g of the title compound, m.p. 114°-116° C.

Workup

  1. temperaturewas heated
  2. temperatureat reflux for ten days
  3. concentrationThe mixture was then concentrated in vacuo
  4. customthe residue chromatographed over silica gel (eluted with 20% ethyl acetate/hexane)

Sources & evidence

ORD record
ord-b20525a2460448ec8ee148133ce23707
Source dataset
uspto-grants-1996_08
Patent number
US05550117

Reaction notes

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