Diethyl Ether → HCID 178496012, compound

HRID 1971137Notes

Reaction equation

HRID 1971137 reaction equation
[C:1]([NH:4][C@@H:5]1[CH2:10][CH2:9][CH2:8][CH2:7][C@@H:6]1[NH:11][C:12]1[C:21]2[C:16](=[CH:17][CH:18]=[C:19]([CH3:22])[CH:20]=2)[N:15]=[C:14]([C:23]([NH:25][CH2:26][CH2:27][O:28][CH3:29])=[O:24])[N:13]=1)(=[NH:3])[CH3:2].C(OCC)(=O)C.[ClH:36].C(OCC)C>C(OCC)(=O)C>[ClH:36].[ClH:36].[C:1]([NH:4][C@@H:5]1[CH2:10][CH2:9][CH2:8][CH2:7][C@@H:6]1[NH:11][C:12]1[C:21]2[C:16](=[CH:17][CH:18]=[C:19]([CH3:22])[CH:20]=2)[N:15]=[C:14]([C:23]([NH:25][CH2:26][CH2:27][O:28][CH3:29])=[O:24])[N:13]=1)(=[NH:3])[CH3:2]

Participants

5

Reactant 3

HCID 3283Diethyl EtherHCID 21866389Hydrogen chloride-ethyl acetateHCID 178496011HCID 178496011, compound

Product 1

HCID 178496012HCID 178496012, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

To a solution of 391 mg of 4-{[(1S,2R)-2-(ethanimidoylamino)cyclohexyl]amino}-N-(2-methoxyethyl)-6-methylquinazolin-2-carboxamide in 5 ml of ethyl acetate, 3 ml of a 4 N hydrogen chloride-ethyl acetate solution was added, and the mixture was stirred for 10 minutes. Then, to the reaction solution, 10 ml of diethyl ether was added, and the deposited substance was collected by filtration, washed with diethyl ether and dried under reduced pressure, whereby 405 mg of a desired compound was obtained as a white powder.

Workup

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

Sources & evidence

ORD record
ord-0616a39cd0014468a43ae6bf211418ac
Source dataset
uspto-grants-2013_04
Patent number
US08431586B2

Reaction notes

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