1,4-Dioxane hydrochloride → HCID 178479026, compound

HRID 2109031Notes

Reaction equation

HRID 2109031 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-1dde7c08dd2a4905a6ffcb4a58680e62
Source dataset
uspto-grants-2009_04
Patent number
US07514449B2

Reaction notes

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