Diethyl Ether → HCID 178496014, compound

HRID 75530Notes

Reaction equation

HRID 75530 reaction equation
[NH2:1][C:2]([NH:6][C@@H:7]1[CH2:12][CH2:11][CH2:10][CH2:9][C@@H:8]1[NH:13][C:14]1[C:23]2[C:18](=[CH:19][CH:20]=[C:21]([CH3:24])[CH:22]=2)[N:17]=[C:16]([C:25]([NH:27][CH2:28][CH2:29][O:30][CH3:31])=[O:26])[N:15]=1)=[N:3][O:4][CH3:5].C(OCC)(=O)C.[ClH:38].C(OCC)C>C(OCC)(=O)C>[ClH:38].[ClH:38].[NH2:1][C:2]([NH:6][C@@H:7]1[CH2:12][CH2:11][CH2:10][CH2:9][C@@H:8]1[NH:13][C:14]1[C:23]2[C:18](=[CH:19][CH:20]=[C:21]([CH3:24])[CH:22]=2)[N:17]=[C:16]([C:25]([NH:27][CH2:28][CH2:29][O:30][CH3:31])=[O:26])[N:15]=1)=[N:3][O:4][CH3:5]

Participants

5

Reactant 3

HCID 3283Diethyl EtherHCID 21866389Hydrogen chloride-ethyl acetateHCID 178496013HCID 178496013, compound

Product 1

HCID 178496014HCID 178496014, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

1.71 g of 4-[((1S,2R)-2-{[amino(methoxyimino)methyl]amino}cyclohexyl)amino]-N-(2-methoxyethyl)-6-methyl quinazolin-2-carboxamide was suspended in 20 ml of ethyl acetate, and 5 ml of a 4 N hydrogen chloride-ethyl acetate solution was added thereto, and the mixture was stirred for 15 minutes. To the reaction solution, 40 ml of diethyl ether was added, and the resulting deposited substance was collected by filtration, washed with diethyl ether and dried under reduced pressure, whereby 2.01 g of a desired compound was obtained as a white powder.

Workup

  1. filtrationwas collected by filtration
  2. washwashed with diethyl ether
  3. customdried under reduced pressure

Sources & evidence

ORD record
ord-f3deb738906c452eb67f70233e81891a
Source dataset
uspto-grants-2014_09
Patent number
US08835446B2

Reaction notes

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