1,4-Dioxane hydrochloride → HCID 69222283, compound

HRID 2061254Notes

Reaction equation

HRID 2061254 reaction equation
[CH:1]1[C:11]2[CH:10]=[CH:9][C:8]3[CH:12]=[CH:13][CH:14]=[CH:15][C:7]=3[C:6](=[C:16]3[CH2:21][CH2:20][N:19]([C:22](=[O:39])[CH2:23][NH:24][C:25]([CH:27]4[CH2:31][CH2:30][CH2:29][N:28]4C(OC(C)(C)C)=O)=[O:26])[CH2:18][CH2:17]3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.[ClH:40].O1CCOCC1>O1CCOCC1>[ClH:40].[CH:1]1[C:11]2[CH:10]=[CH:9][C:8]3[CH:12]=[CH:13][CH:14]=[CH:15][C:7]=3[C:6](=[C:16]3[CH2:21][CH2:20][N:19]([C:22](=[O:39])[CH2:23][NH:24][C:25]([C@H:27]4[CH2:31][CH2:30][CH2:29][NH:28]4)=[O:26])[CH2:18][CH2:17]3)[C:5]=2[CH:4]=[CH:3][CH:2]=1

Participants

4

Reactant 2

HCID 204431481,4-Dioxane hydrochloride4×HCID 68421687HCID 68421687, compound

Product 1

HCID 69222283HCID 69222283, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

854 mg (1.62 mmol) of the compound obtained in step 1 described above was dissolved in 20 ml of 1,4-dioxane. 2 ml of 4 N hydrochloric acid/1,4-dioxane was added to the obtained solution under cooling with ice, and they were stirred at room temperature for 2.5 hours. The reaction mixture was cooled with ice, 5 ml of 4 N hydrochloric acid/1,4-dioxane was added thereto, and they were stirred at room temperature for 2 hours. 2.5 ml of 4 N hydrochloric acid/1,4-dioxane was added to the reaction mixture under cooling with ice. After stirring at room temperature for 1 hour, 7.5 ml of 4 N hydrochloric acid/1,4-dioxane was added to the reaction mixture, and they were stirred at room temperature for 2 hours. The solvent was concentrated under reduced pressure. Diethyl ether was added to the residue, and crystals thus formed were taken by the filtration to obtain the title compound.

Workup

  1. temperatureunder cooling with ice, and they
  2. additionwas added
  3. stirringthey were stirred at room temperature for 2 hours
  4. temperatureunder cooling with ice
  5. stirringAfter stirring at room temperature for 1 hour
  6. stirringwere stirred at room temperature for 2 hours
  7. concentrationThe solvent was concentrated under reduced pressure
  8. additionDiethyl ether was added to the residue, and crystals
  9. customthus formed
  10. filtrationwere taken by the filtration

Sources & evidence

ORD record
ord-6e18ebfe99514fef834b216eb6cb6c30
Source dataset
uspto-grants-2012_10
Patent number
US08278329B2

Reaction notes

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