1,4-Dioxane hydrochloride → HCID 66717443, compound

HRID 241249Notes

Reaction equation

HRID 241249 reaction equation
C([O:5][C:6](=[O:46])[CH2:7][N:8](C(OC(C)(C)C)=O)[C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([CH:15]([CH2:26][C:27]2[N:28]=[N:29][C:30]([C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)=[CH:31][CH:32]=2)[NH:16][S:17]([C:20]2[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=2)(=[O:19])=[O:18])[N:10]=1)(C)(C)C.[ClH:47].O1CCOCC1>C(Cl)Cl>[ClH:47].[C:33]1([C:30]2[N:29]=[N:28][C:27]([CH2:26][CH:15]([NH:16][S:17]([C:20]3[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=3)(=[O:19])=[O:18])[C:11]3[N:10]=[C:9]([NH:8][CH2:7][C:6]([OH:46])=[O:5])[CH:14]=[CH:13][CH:12]=3)=[CH:32][CH:31]=2)[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1

Participants

4

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 86651766HCID 86651766, compound

Product 1

HCID 66717443HCID 66717443, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

To a solution of tert-butyl(tert-butoxycarbonyl{6-[(6-phenylpyridazin-3-ylmethyl)(pyridin-3-ylsulfonyl)aminomethyl]pyridin-2-yl}amino)acetate (150 mg, 0.232 mmol) obtained in Example 1-(b) in methylene chloride (9.2 ml) was added a 4N hydrogen chloride/1,4-dioxane solution (2.3 ml), and the mixture was left at room temperature for 23 hours. After completion of the reaction, the reaction solution was concentrated under reduced pressure to afford the title compound (144 mg) substantially quantitatively as a white solid.

Workup

  1. customAfter completion of the reaction
  2. concentrationthe reaction solution was concentrated under reduced pressure

Sources & evidence

ORD record
ord-f8faf236597b472d946d1577db4b9b71
Source dataset
uspto-grants-2014_02
Patent number
US08648097B2

Reaction notes

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