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 1183089Notes

Reaction equation

HRID 1183089 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-abe31ad30f9b40e6a1a6346784fa6c60
Source dataset
uspto-grants-2014_03
Patent number
US08664217B2

Reaction notes

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