1,4-Dioxane hydrochloride → HCID 68489011, compound

HRID 389040Notes

Reaction equation

HRID 389040 reaction equation
Cl.O1CCOCC1.[CH2:8]([O:10][C:11]([CH2:13][CH2:14][C:15]1[S:16][C:17]2[CH:18]=[CH:19][C:20]3[CH:41]=[CH:40][CH:39]=[CH:38][C:21]=3[C:22](=[C:25]3[CH2:30][CH2:29][N:28](C(OC(C)(C)C)=O)[CH2:27][CH2:26]3)[C:23]=2[CH:24]=1)=[O:12])[CH3:9]>O1CCOCC1>[NH:28]1[CH2:29][CH2:30][C:25](=[C:22]2[C:21]3[CH:38]=[CH:39][CH:40]=[CH:41][C:20]=3[CH:19]=[CH:18][C:17]3[S:16][C:15]([CH2:14][CH2:13][C:11]([O:10][CH2:8][CH3:9])=[O:12])=[CH:24][C:23]2=3)[CH2:26][CH2:27]1

Participants

4

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 68752009HCID 68752009, compound

Product 1

HCID 68489011HCID 68489011, compoundYield 88%

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

Hydrogen chloride-dioxane (7.5 mL, equivalent to 30 mmol of hydrogen chloride) was added to a dioxane (30 mL) solution of the compound obtained in Example 35 (2.9 g, 6.0 mmol), and the mixture was stirred at room temperature for 5 hours. The solvents were distilled off under a reduced pressure, and the residue was purified by column chromatography (chloroform-methanol=19:1), to give 2.0 g (88%) of the captioned compound in the form of an oily product.

Workup

  1. distillationThe solvents were distilled off under a reduced pressure
  2. customthe residue was purified by column chromatography (chloroform-methanol=19:1)

Sources & evidence

ORD record
ord-ed29d07989ac4cd5b056df173c16f1b0
Source dataset
uspto-grants-2013_02
Patent number
US08377967B2

Reaction notes

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