Alfentanil hydrochloride → Alfentanil

HRID 1792143Notes

Reaction equation

HRID 1792143 reaction equation
[CH3:1][CH2:2][C:3]([N:5]([C:12]1([CH2:28][O:29][CH3:30])[CH2:17][CH2:16][N:15]([CH2:18][CH2:19][N:20]2[N:25]=[N:24][N:23]([CH2:26][CH3:27])[C:21]2=[O:22])[CH2:14][CH2:13]1)[C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1)=[O:4].Cl>O>[CH3:1][CH2:2][C:3]([N:5]([C:12]1([CH2:28][O:29][CH3:30])[CH2:13][CH2:14][N:15]([CH2:18][CH2:19][N:20]2[N:25]=[N:24][N:23]([CH2:26][CH3:27])[C:21]2=[O:22])[CH2:16][CH2:17]1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:4]

Participants

3

Reactant 1

HCID 64761Alfentanil hydrochloride

Product 1

HCID 51263Alfentanil

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

The alfentanil HCl obtained from step 7 is recrystallized from an HCl solution to give the final product as follows. 60.5 g of alfentanil HCl is placed into 2.5× amount of water (151 g H2O). To this is added 5.2 g activated charcoal and 10.4 g filtration aid (diatomaceous earth). Then 15.1 mL concentrated HCl is added (0.25 mL/g alfentanil HCl) and this is stirred until a slurry forms. This is followed by addition of 1 mL 1 N HCl/g alfentanil HCl (60.5 mL of 1 N HCl in this Example). This is chilled for over 2 hours and then filtered. The product is dried at approximately 40–55° C. until it is a constant weight. This final product is a monohydrate form of alfentanil HCl.

Workup

  1. customThe alfentanil HCl obtained from step 7 is recrystallized from an HCl solution
  2. customto give the final product
  3. additionTo this is added 5.2 g
  4. filtrationcharcoal and 10.4 g filtration aid (diatomaceous earth)
  5. additionThen 15.1 mL concentrated HCl is added (0.25 mL/g alfentanil HCl)
  6. additionThis is followed by addition of 1 mL 1 N HCl/g alfentanil HCl (60.5 mL of 1 N HCl in this Example)
  7. temperatureThis is chilled for over 2 hours
  8. filtrationfiltered
  9. customThe product is dried at approximately 40–55° C. until it

Sources & evidence

ORD record
ord-c3f077b560234ffeaa73dcf109fde939
Source dataset
uspto-grants-2006_07
Patent number
US07074935B2

Reaction notes

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