1,2-Ethanediamine, N1,N1-bis(1-methylethyl)- → HCID 53986383, compound

HRID 1952808Notes

Reaction equation

[CH:1]([N:4]([CH:8]([CH3:10])[CH3:9])[CH2:5][CH2:6][NH2:7])([CH3:3])[CH3:2].C(N(CC)CCN[C:17]([O:19][CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=1[N:27]([CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH3:47])[CH:28]=[O:29])=[O:18])C>C(Cl)(Cl)Cl>[CH:1]([N:4]([CH:8]([CH3:10])[CH3:9])[CH2:5][CH2:6][NH:7][C:17]([O:19][CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=1[N:27]([CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH3:47])[CH:28]=[O:29])=[O:18])([CH3:3])[CH3:2]

Participants

Conditions

Temperature: 70 °C

Procedure

N,N-Diisopropylethylenediamine (0.79 g) was added to the intermediate (a) (2.62g) obtained in Example 28. After being stirred for 2 hours at 70° C., the reaction mixture, with chloroform added thereto, was washed with 1N sodium hydroxide aqueous solution and saturated brine successively, dried over sodium sulfate anhydride, and then filtrated. The solvent was evaporated out and the residue was purified by silica gel column chromatography (silica gel 85 g, chloroform:methanol=100:1), thereby yielding 1.45 g of the aimed compound as white solid.

Workup

washwas washed with 1N sodium hydroxide aqueous solution and saturated brine successively
dry with materialdried over sodium sulfate anhydride
filtrationfiltrated
customThe solvent was evaporated out
customthe residue was purified by silica gel column chromatography (silica gel 85 g, chloroform:methanol=100:1)

Sources & evidence

ORD record: ord-2f313e17b67044f0876bf7fa1656f5e5
Source dataset: uspto-grants-2000_09
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US06114325

Reaction notes

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