Hydrochloride methanol → HCID 178496799, compound

HRID 703389Notes

Reaction equation

HRID 703389 reaction equation
Cl.Cl.Cl.[NH2:4][CH2:5][CH2:6][CH2:7][NH:8][CH2:9][CH2:10][CH2:11][CH2:12][NH:13][C:14](=[O:32])[CH:15]([NH:17][C:18](=[O:31])[CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][NH:27][C:28]([NH2:30])=[NH:29])[OH:16].Cl.[CH3:34]O>CO>[NH2:4][CH2:5][CH2:6][CH2:7][NH:8][CH2:9][CH2:10][CH2:11][CH2:12][NH:13][C:14](=[O:32])[CH:15]([NH:17][C:18](=[O:31])[CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][NH:27][C:28]([NH2:30])=[NH:29])[O:16][CH3:34]

Participants

4

Reactant 2

HCID 21893726Hydrochloride methanolHCID 178478606HCID 178478606, compound

Product 1

HCID 178496799HCID 178496799, compoundYield 65%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a solution of 160 mg (0.31 mmole) of N-[4-(3-aminopropyl)aminobutyl]-2-(9-guanidinononanamido)-2-hydroxyethanamide trihydrochloride in 3.2 ml of anhydrous methanol was added 0.32 ml of 2N hydrogen chloride-methanol. The mixture was stirred overnight at room temperature. The reaction mixture was concentrated under reduced pressure and the resulting white powder was purified in a manner as that in Example 7, using CM-Sephadex® C-25 (Na-type) and Sephadex® LH-20 to yield 107 mg (65% yield) of a white powder of N-[4-(3-aminopropyl)aminobutyl]-2-(9-guanidinonoanamido)-2-methoxyethanamide trihydrochloride.

Workup

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customthe resulting white powder was purified in a manner as that in Example 7

Sources & evidence

ORD record
ord-6c26b4048f92434ca0871a0b27b5bc5e
Source dataset
uspto-grants-1991_01
Patent number
US04983328

Reaction notes

Loading…