Hydrogen chloride-ethyl acetate → 1-Ethyl-3,3,5-trimethyl-7-[3-(2-pyridin-3-ylethylamino)propoxy]-1,5-dihydrobenzo[b][1,4]diazepine-2, 4-dione dihydrochloride

HRID 2196072Notes

Reaction equation

HRID 2196072 reaction equation
C(OC(=O)C)C.[ClH:7].[CH2:8]([N:10]1[C:16](=[O:17])[C:15]([CH3:19])([CH3:18])[C:14](=[O:20])[N:13]([CH3:21])[C:12]2[CH:22]=[C:23]([O:26][CH2:27][CH2:28][CH2:29][NH:30][CH2:31][CH2:32][C:33]3[CH:34]=[N:35][CH:36]=[CH:37][CH:38]=3)[CH:24]=[CH:25][C:11]1=2)[CH3:9]>C(OCC)(=O)C>[ClH:7].[ClH:7].[CH2:8]([N:10]1[C:16](=[O:17])[C:15]([CH3:19])([CH3:18])[C:14](=[O:20])[N:13]([CH3:21])[C:12]2[CH:22]=[C:23]([O:26][CH2:27][CH2:28][CH2:29][NH:30][CH2:31][CH2:32][C:33]3[CH:34]=[N:35][CH:36]=[CH:37][CH:38]=3)[CH:24]=[CH:25][C:11]1=2)[CH3:9]

Participants

4

Reactant 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 686730021-Ethyl-3,3,5-trimethyl-7-[3-(2-pyridin-3-ylethylamino) propoxy]-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione

Product 1

HCID 686735041-Ethyl-3,3,5-trimethyl-7-[3-(2-pyridin-3-ylethylamino)propoxy]-1,5-dihydrobenzo[b][1,4]diazepine-2, 4-dione dihydrochlorideYield 85%

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

A 4N-hydrogen chloride ethyl acetate solution (0.37 ml) was added to an ethyl acetate solution (10 ml) of 1-ethyl-3,3,5-trimethyl-7-[3-(2-pyridin-3-ylethylamino)propoxy]-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione (207 mg, 0.49 mmol), and stirred for 30 minutes at room temperature. The precipitated insoluble matter was collected by filtration, washed with ethyl acetate, and dried to thereby obtain 208 mg (yield: 85%) of 1-ethyl-3,3,5-trimethyl-7-[3-(2-pyridin-3-ylethylamino)propoxy]-1,5-dihydrobenzo[b][1,4]diazepine-2, 4-dione dihydrochloride as a pale yellow amorphous solid.

Workup

  1. filtrationThe precipitated insoluble matter was collected by filtration
  2. washwashed with ethyl acetate
  3. customdried

Sources & evidence

ORD record
ord-e73677c7559d4caf8f696b95072c7bc3
Source dataset
uspto-grants-2012_12
Patent number
US08338406B2

Reaction notes

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