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1,4-Dioxane hydrochloride → HCID 69001602, compound

HRID 1909631
Notes
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Reaction equation

HRID 1909631 reaction equation
C([O:5][C:6](=[O:29])[CH2:7][N:8]1[CH2:12][CH2:11][CH2:10][C@@H:9]1[CH2:13][O:14][C:15]1[CH:20]=[CH:19][C:18]([O:21][C:22]2[CH:27]=[CH:26][C:25]([Cl:28])=[CH:24][CH:23]=2)=[CH:17][CH:16]=1)(C)(C)C.Cl.O1CCOCC1>>[ClH:28].[Cl:28][C:25]1[CH:26]=[CH:27][C:22]([O:21][C:18]2[CH:19]=[CH:20][C:15]([O:14][CH2:13][C@H:9]3[CH2:10][CH2:11][CH2:12][N:8]3[CH2:7][C:6]([OH:29])=[O:5])=[CH:16][CH:17]=2)=[CH:23][CH:24]=1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

3

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 68999682HCID 68999682, compound

Product 1

HCID 69001602HCID 69001602, compoundYield 173.3%

Conditions

Temperature
60 °C

Procedure

To the product from step 5 (0.60 g, 1.42 mmol) was added a 1:1 mixture of concentrated HCl/dioxane (28 mL). The resulting solution was stirred at 60° C. for 4 h. The solvent was removed in vacuo. The crude product was triturated with ether and dried under reduced pressure to afford the title compound (0.49 g, 52%) as a white solid.

Workup

  1. customThe solvent was removed in vacuo
  • customThe crude product was triturated with ether
  • customdried under reduced pressure
  • Sources & evidence

    ORD record
    ord-7e2c9cae20214a0986aee2192eddf3f8
    Source dataset
    uspto-grants-2013_12
    DOI
    10.6084/m9.figshare.5104873.v1
    Patent number
    US08598359B2

    Reaction notes

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    On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes