1,4-Dioxane hydrochloride → HCID 86614602, compound

HRID 901969Notes

Reaction equation

HRID 901969 reaction equation
[F:1][C:2]([F:58])([F:57])[C:3]1[CH:4]=[C:5]([CH:50]=[C:51]([C:53]([F:56])([F:55])[F:54])[CH:52]=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][O:46][CH2:47][CH2:48][OH:49])[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].Cl.O1CCOCC1>C(Cl)Cl>[ClH:20].[F:56][C:53]([F:54])([F:55])[C:51]1[CH:50]=[C:5]([CH:4]=[C:3]([C:2]([F:58])([F:57])[F:1])[CH:52]=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][O:46][CH2:47][CH2:48][OH:49])[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

4

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 86614603HCID 86614603, compound

Product 1

HCID 86614602HCID 86614602, compoundYield 179.5%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

68.2 mg (0.079 mmol) of the 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-[2-(2-hydroxyethoxy)ethyl]-N-methylacetamide was dissolved in 5 mL of methylene chloride and 0.2 mL of 4N hydrochloric acid-dioxane solution was added dropwise thereto. The solvent was distilled off under reduced pressure and the thus obtained amorphous matter was collected by filtration by adding n-hexane to obtain 63.6 mg (yield: 89%) of the title compound as a white solid.

Workup

  1. distillationThe solvent was distilled off under reduced pressure
  2. filtrationthe thus obtained amorphous matter was collected by filtration
  3. additionby adding n-hexane

Sources & evidence

ORD record
ord-984adb0832ce4ae9875fa7517b5fea59
Source dataset
uspto-grants-2008_04
Patent number
US07365067B2

Reaction notes

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