HCID 86614601, compound → HCID 86614600, compound

HRID 901968Notes

Reaction equation

HRID 901968 reaction equation
[F:1][C:2]([F:57])([F:56])[C:3]1[CH:4]=[C:5]([CH:49]=[C:50]([C:52]([F:55])([F:54])[F:53])[CH:51]=1)[C:6]([N:8]1[CH2:13][CH2:12][O:11][C@:10]([CH2:22][CH2:23][N:24]2[CH2:29][CH2:28][C:27]3([C:37]4[C:32](=[CH:33][CH:34]=[CH:35][CH:36]=4)[CH2:31][C@@H:30]3[O:38][CH2:39][C:40]([N:42]([CH2:44][CH2:45][CH2:46][CH2:47][OH:48])[CH3:43])=[O:41])[CH2:26][CH2:25]2)([C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[C:16]([Cl:21])[CH:15]=2)[CH2:9]1)=[O:7]>C(OCC)(=O)C>[ClH:20].[F:55][C:52]([F:53])([F:54])[C:50]1[CH:49]=[C:5]([CH:4]=[C:3]([C:2]([F:57])([F:56])[F:1])[CH:51]=1)[C:6]([N:8]1[CH2:13][CH2:12][O:11][C@:10]([CH2:22][CH2:23][N:24]2[CH2:29][CH2:28][C:27]3([C:37]4[C:32](=[CH:33][CH:34]=[CH:35][CH:36]=4)[CH2:31][C@@H:30]3[O:38][CH2:39][C:40]([N:42]([CH2:44][CH2:45][CH2:46][CH2:47][OH:48])[CH3:43])=[O:41])[CH2:26][CH2:25]2)([C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[C:16]([Cl:21])[CH:15]=2)[CH2:9]1)=[O:7]

Participants

3

Reactant 1

HCID 86614601HCID 86614601, compound

Product 1

HCID 86614600HCID 86614600, compoundYield 96%

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

The thus obtained 2-[((2S)-1′-{2-[(2R)-4-[3,5-bis(trifluoromethyl)benzoyl]-2-(3,4-dichlorophenyl)morpholin-2-yl]ethyl}-2,3-dihydrospiro[indene-1,4′-piperidin]-2-yl)oxy]-N-(4-hydroxybutyl)-N-methylacetamide was dissolved in 20 mL of ethyl acetate and the mixture was extracted with 20 mL of 1N aqueous hydrochloric acid solution. After the ethyl acetate layer was dried over anhydrous sodium sulfate, the solvent was distilled off under reduced pressure. The thus obtained amorphous matter was collected by filtration by adding n-hexane to obtain 1.89 g (yield: 96%) of the title compound as a white solid.

Workup

  1. extractionthe mixture was extracted with 20 mL of 1N aqueous hydrochloric acid solution
  2. dry with materialAfter the ethyl acetate layer was dried over anhydrous sodium sulfate
  3. distillationthe solvent was distilled off under reduced pressure
  4. filtrationThe thus obtained amorphous matter was collected by filtration
  5. additionby adding n-hexane

Sources & evidence

ORD record
ord-dbbcad890c924c8b93ae41a49e0c4215
Source dataset
uspto-grants-2008_04
Patent number
US07365067B2

Reaction notes

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