Hydrochloric Acid → HCID 69522544, compound

HRID 856569Notes

Reaction equation

HRID 856569 reaction equation
C(OC[CH2:6][N:7]1[CH:11]=[CH:10][N:9]=[C:8]1[CH2:12][S:13]([C:15]1[CH:20]=[CH:19][C:18]([NH:21][C:22]([C:24]2[CH2:25][CH2:26][N:27]([CH2:49][CH:50]([CH3:52])[CH3:51])[C:28]3[CH:34]=[CH:33][C:32]([C:35]4[CH:40]=[CH:39][C:38]([O:41][CH2:42][CH2:43][O:44][CH2:45][CH2:46][CH2:47][CH3:48])=[CH:37][CH:36]=4)=[CH:31][C:29]=3[CH:30]=2)=[O:23])=[CH:17][CH:16]=1)=[O:14])(=O)C.[OH-:53].[Na+].Cl.[CH2:56]([OH:58])C>>[CH2:45]([O:44][CH2:43][CH2:42][O:41][C:38]1[CH:37]=[CH:36][C:35]([C:32]2[CH:33]=[CH:34][C:28]3[N:27]([CH2:49][CH:50]([CH3:52])[CH3:51])[CH2:26][CH2:25][C:24]([C:22]([NH:21][C:18]4[CH:19]=[CH:20][C:15]([S:13]([CH2:12][C:8]5[N:7]([CH2:6][C:56]([OH:58])=[O:53])[CH:11]=[CH:10][N:9]=5)=[O:14])=[CH:16][CH:17]=4)=[O:23])=[CH:30][C:29]=3[CH:31]=2)=[CH:40][CH:39]=1)[CH2:46][CH2:47][CH3:48]

Participants

5

Reactant 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 14798Sodium HydroxideHCID 69521589HCID 69521589, compound

Product 1

HCID 69522544HCID 69522544, compound

Procedure

To a solution of [2-[[[4-[[[7-[4-(2-butoxyethoxy)phenyl]-1-isobutyl-2,3-dihydro-1H-1-benzazepin-4-yl]carbonyl]amino]phenyl]sulfinyl]methyl]-1H-imidazol-1-yl]ethyl acetate (85 mg) in ethanol (5 ml) was added 1N aqueous solution of sodium hydroxide (0.14 ml) at room temperature. The mixture was stirred at room temperature for 1 hour, 1N hydrochloric acid (0.14 ml) was added to the mixture, and the mixture was concentrated under reduced pressure. To the residue was added 2-propanol, and the precipitated crystals were collected by filtration. The crystals were washed with 2-propanol and diisopropyl ether, to give [2-[[[4-[[[7-[4-(2-butoxyethoxy) phenyl]-1-isobutyl-2,3-dihydro-1H-1-benzazepin-4-yl]carbonyl]amino]phenyl]sulfinyl]methyl]-1H-imidazol-1-yl]acetic acid (Preparation of Compound 412) (65.7 mg) as yellow crystals.

Workup

  1. concentrationthe mixture was concentrated under reduced pressure
  2. additionTo the residue was added 2-propanol
  3. filtrationthe precipitated crystals were collected by filtration
  4. washThe crystals were washed with 2-propanol and diisopropyl ether

Sources & evidence

ORD record
ord-7918523c6a9848f8a5aa675875b2b254
Source dataset
uspto-grants-2007_08
Patent number
US07262185B2

Reaction notes

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