Diethyl Ether → HCID 86650786, compound

HRID 1893580Notes

Reaction equation

HRID 1893580 reaction equation
[C:1]([C:3]1[CH:4]=[CH:5][C:6]([CH3:41])=[C:7]([N:9]([CH2:27][C:28]([N:30]([N:32]2[CH2:40][C:39]3[C:34](=[CH:35][CH:36]=[CH:37][CH:38]=3)[CH2:33]2)[CH3:31])=[O:29])[CH2:10][C:11]([NH:13][CH2:14][CH2:15][N:16](C(OC(C)(C)C)=O)[CH:17]([CH3:19])[CH3:18])=[O:12])[CH:8]=1)#[N:2].[ClH:42].O1CCOCC1.C(OCC)C>ClCCl>[ClH:42].[ClH:42].[C:1]([C:3]1[CH:4]=[CH:5][C:6]([CH3:41])=[C:7]([N:9]([CH2:27][C:28]([N:30]([N:32]2[CH2:33][C:34]3[C:39](=[CH:38][CH:37]=[CH:36][CH:35]=3)[CH2:40]2)[CH3:31])=[O:29])[CH2:10][C:11]([NH:13][CH2:14][CH2:15][NH:16][CH:17]([CH3:18])[CH3:19])=[O:12])[CH:8]=1)#[N:2]

Participants

5

Reactant 3

HCID 3283Diethyl EtherHCID 204431481,4-Dioxane hydrochlorideHCID 86650785HCID 86650785, compound

Product 1

HCID 86650786HCID 86650786, compoundYield 97.3%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

The compound (2.81 g, 4.99 mmol) obtained in step B was dissolved in dichloromethane (15 ml), 4N hydrochloric acid-dioxane solution (15 ml, 60 mmol) was added at room temperature, and the mixture was stirred at the same temperature for 2 hr. Diethyl ether was added to the reaction mixture, and the precipitated solid was collected by filtration, washed with diethyl ether, and dried under reduced pressure to give the title compound (2.60 g, yield 97%) as a colorless solid.

Workup

  1. filtrationthe precipitated solid was collected by filtration
  2. washwashed with diethyl ether
  3. customdried under reduced pressure

Sources & evidence

ORD record
ord-17fab578a2a943e5863c6497b008dc9c
Source dataset
uspto-grants-2013_08
Patent number
US08513235B2

Reaction notes

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