1,4-Dioxane hydrochloride → HCID 66941300, compound

HRID 348684Notes

Reaction equation

HRID 348684 reaction equation
[CH2:1]([O:8][C:9](=[O:48])[N:10]([CH2:17][C:18]1[CH:23]=[CH:22][C:21]([NH:24][C:25](=[O:47])[C:26]2[CH:31]=[CH:30][C:29]([CH2:32][N:33](C(OC(C)(C)C)=O)[CH2:34][C:35]3[NH:36][CH:37]=[CH:38][N:39]=3)=[CH:28][CH:27]=2)=[CH:20][CH:19]=1)[CH:11]1[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.O1CCOCC1>CO>[CH2:1]([O:8][C:9](=[O:48])[N:10]([CH:11]1[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16]1)[CH2:17][C:18]1[CH:19]=[CH:20][C:21]([NH:24][C:25](=[O:47])[C:26]2[CH:31]=[CH:30][C:29]([CH2:32][NH:33][CH2:34][C:35]3[NH:39][CH:38]=[CH:37][N:36]=3)=[CH:28][CH:27]=2)=[CH:22][CH:23]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

4

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 66941970HCID 66941970, compound

Product 1

HCID 66941300HCID 66941300, compoundYield 96.1%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

The compound (1.82 g) obtained in Example 87-3 was dissolved in methanol (18 ml) and then added with a 4 mol/l hydrogen chloride/dioxane solution (18 ml), followed by stirring at room temperature for 2 hours. After the reaction, the solvent was distilled off. Then, the residue was adjusted to pH 11 with a 1 mol/l sodium hydroxide aqueous solution and extracted with chloroform, followed by drying with anhydrous magnesium sulfate. Subsequently, the solvent was distilled off, thereby obtaining the subject compound (1.48 g) as a white solid.

Workup

  1. customAfter the reaction
  2. distillationthe solvent was distilled off
  3. extractionextracted with chloroform
  4. dry with materialby drying with anhydrous magnesium sulfate
  5. distillationSubsequently, the solvent was distilled off

Sources & evidence

ORD record
ord-fb2f2fb5e1f34d97bb25e4246ece44b5
Source dataset
uspto-grants-2007_02
Patent number
US07176227B2

Reaction notes

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