1,4-Dioxane hydrochloride → HCID 66941300, compound

HRID 1173936Notes

Reaction equation

HRID 1173936 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-a1114de3bbd143a797044fb8c58a639a
Source dataset
uspto-grants-2010_11
Patent number
US07833991B2

Reaction notes

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