2-Hydrazino-delta-2-imidazoline hydrobromide → HCID 88183062, compound

HRID 1936739Notes

Reaction equation

HRID 1936739 reaction equation
[NH:1]1[CH2:5][CH2:4][N:3]=[C:2]1[NH:6][N:7]=[C:8]([CH3:35])[CH2:9][CH2:10][C:11]1[CH:16]=[CH:15][C:14]([O:17][CH2:18][CH2:19][C@@H:20]([C:32]([OH:34])=[O:33])[NH:21][C:22]([O:24][CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)=[O:23])=[CH:13][CH:12]=1.Br.N1[CH2:41][CH2:40]N=C1NN>C(O)CCC>[NH:3]1[CH2:4][CH2:5][N:1]=[C:2]1[NH:6][N:7]=[C:8]([CH3:35])[CH2:9][CH2:10][C:11]1[CH:16]=[CH:15][C:14]([O:17][CH2:18][CH2:19][C@@H:20]([C:32]([O:34][CH2:40][CH3:41])=[O:33])[NH:21][C:22]([O:24][CH2:25][C:26]2[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=2)=[O:23])=[CH:13][CH:12]=1

Participants

4

Reactant 2

HCID 30850992-Hydrazino-delta-2-imidazoline hydrobromideHCID 86758080HCID 86758080, compound

Product 1

HCID 88183062HCID 88183062, compoundYield 109.9%

Reagents, catalysts & solvents 1

HCID 2631-ButanolSolvent

Conditions

Temperature
110 °C

Procedure

The mixture constituted by 430 mg of the ketone prepared in Stage A, 549 mg of 4,5-dihydro-1H-imidazol-2-yl-hydrazine hydrobromide in 20 ml of butanol is heated at the temperature of 110° C. for 2 hours then evaporated under reduced pressure until 1.1 g of crude product is obtained which is purified by chromatography (Kieselgel 60, 40-63 μm) eluting with a dichloromethane/methanol mixture 90/10. 500 mg of expected product is obtained.

Workup

  1. customthen evaporated under reduced pressure until 1.1 g of crude product
  2. customis obtained which
  3. customis purified by chromatography (Kieselgel 60, 40-63 μm)
  4. washeluting with a dichloromethane/methanol mixture 90/10

Sources & evidence

ORD record
ord-c3cb8f736dee4a9d85dfaab43c6507fb
Source dataset
uspto-grants-2002_05
Patent number
US06391904B1

Reaction notes

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