Chloroform → HCID 12582644, compound

HRID 1633062Notes

Reaction equation

HRID 1633062 reaction equation
Cl[C:2]1[N:7]=[N:6][C:5]2[CH2:8][CH2:9][N:10]([C:12](=[O:17])[CH2:13][CH2:14][CH:15]=[CH2:16])[CH2:11][C:4]=2[CH:3]=1.C(Cl)(Cl)Cl.O.[NH2:23][NH2:24]>>[NH:23]([C:2]1[N:7]=[N:6][C:5]2[CH2:8][CH2:9][N:10]([C:12](=[O:17])[CH2:13][CH2:14][CH:15]=[CH2:16])[CH2:11][C:4]=2[CH:3]=1)[NH2:24]

Participants

4

Reactant 3

HCID 6212ChloroformHCID 24654Hydrazine hydrate (1:1)HCID 20441621HCID 20441621, compound

Product 1

HCID 12582644HCID 12582644, compound

Procedure

12.3 g of 3-chloro-5,6,7,8-tetrahydro-6-(4-pentenoyl)pyrido[4,3-c]pyridazine are stirred in 40 cc of hydrazine hydrate at a bath temperature of 90° for 3 hours. The mixture is cooled with ice, 100 cc of chloroform are added, and the excess hydrazine is separated. Upon concentrating the chloroform phase, the crude title compound is obtained as an oil. This is converted to bis[3-hydrazino-5,6,7,8-tetrahydro-6-(4-pentenoyl)pyrido[4,3-c]pyridazine]trisfumarate by boiling with 4 g of fumaric acid in 50 cc of absolute ethanol. M.P. 132°-134° (decomp., from absolute ethanol).

Workup

  1. additionare added
  2. customthe excess hydrazine is separated
  3. concentrationUpon concentrating the chloroform phase

Sources & evidence

ORD record
ord-37a173bc2e214279b49517f86eef10f7
Source dataset
uspto-grants-1984_10
Patent number
US04478837

Reaction notes

Loading…