1,4-Dioxane hydrochloride → HCID 178479026, compound

HRID 16683Notes

Reaction equation

HRID 16683 reaction equation
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][C:9]([C:11]2[O:19][C:18]3[C:13](=[N:14][C:15]([NH:20]C(=O)OC(C)(C)C)=[CH:16][CH:17]=3)[C:12]=2[NH:28][C:29]([C@H:31]2[CH2:36][CH2:35][C@H:34]([N:37]3[CH2:42][CH2:41][O:40][CH2:39][C:38]3=[O:43])[CH2:33][CH2:32]2)=[O:30])=[O:10])=[N:6][CH:7]=1.Cl.O1CCOCC1>CO>[ClH:1].[NH2:20][C:15]1[N:14]=[C:13]2[C:12]([NH:28][C:29]([C@H:31]3[CH2:36][CH2:35][C@H:34]([N:37]4[CH2:42][CH2:41][O:40][CH2:39][C:38]4=[O:43])[CH2:33][CH2:32]3)=[O:30])=[C:11]([C:9]([NH:8][C:5]3[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][N:6]=3)=[O:10])[O:19][C:18]2=[CH:17][CH:16]=1

Participants

4

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 178452647HCID 178452647, compound

Product 1

HCID 178479026HCID 178479026, compoundYield 187.8%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

t-Butyl [2-{[(5-Chloropyridin-2-yl)amino]carbonyl}-3-({[trans-4-(3-oxomorpholin-4-yl)cyclohexyl]carbonyl}amino)furo[3,2-b]pyridin-5-yl]carbamate (5.55 g) obtained in Example 94 is suspended in methanol (20 ml), and thereto is added 4N hydrogen chloride-dioxane solution (50 ml) under ice-cooling. The mixture is stirred at room temperature for 8 hours. The reaction solution is concentrated under reduced pressure and the resulting residue is suspended in diethyl ether. The precipitates are collected by filtration to give the title compound (4.67 g).

Workup

  1. temperaturecooling
  2. concentrationThe reaction solution is concentrated under reduced pressure
  3. filtrationThe precipitates are collected by filtration

Sources & evidence

ORD record
ord-c36f850680bb4600a71400bcc7141e49
Source dataset
uspto-grants-2010_06
Patent number
US07737161B2

Reaction notes

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