Hydrochloric Acid → HCID 14610428, compound

HRID 1005688Notes

Reaction equation

HRID 1005688 reaction equation
C(OC([NH:8][CH2:9][CH2:10][C:11]1[CH:12]=[C:13]([NH:17][C:18]([O:20][CH2:21][CH3:22])=[O:19])[CH:14]=[CH:15][CH:16]=1)=O)(C)(C)C.[ClH:23]>C(O)C>[ClH:23].[CH2:21]([O:20][C:18]([NH:17][C:13]1[CH:12]=[C:11]([CH:16]=[CH:15][CH:14]=1)[CH2:10][CH2:9][NH2:8])=[O:19])[CH3:22]

Participants

4

Reactant 2

HCID 313Hydrochloric Acid3×HCID 22674139HCID 22674139, compound

Product 1

HCID 14610428HCID 14610428, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent3×

Procedure

In ethanol (15 ml) was dissolved 14.96 g of 3-(2-t-butoxycarbonylaminoethyl)-ethoxycarbonylaminobenzene (Preparation Example 36). Under ice-cooling, hydrochloric acid (15 ml) was added thereto, followed by stirring at room temperature for 20 minutes. Hydrochloric acid (12 ml) and ethanol (15 ml) were further added thereto, followed by stirring at room temperature for 20 minutes. Then, hydrochloric acid (20 ml) and ethanol (30 ml) were further added thereto, followed by stirring at room temperature for 30 minutes. The solvent was evaporated (azeotropic distillation with toluene), to give the title compound (11.99 g) as pale yellow crystals.

Workup

  1. temperatureUnder ice-cooling
  2. stirringby stirring at room temperature for 20 minutes
  3. stirringby stirring at room temperature for 30 minutes
  4. customThe solvent was evaporated
  5. distillation(azeotropic distillation with toluene)

Sources & evidence

ORD record
ord-2d1d35034da64db88649745f79e740e1
Source dataset
uspto-grants-2004_09
Patent number
US06787534B2

Reaction notes

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