1,4-Dioxane hydrochloride → HCID 22675293, compound

HRID 1006071Notes

Reaction equation

HRID 1006071 reaction equation
O1CCOCC1.[ClH:7].C(OC([NH:15][C:16]1[CH:21]=[CH:20][C:19]([CH2:22][CH2:23][N:24]2[CH2:29][CH2:28][CH:27]([CH2:30][C:31]3[CH:36]=[C:35]([O:37][CH3:38])[CH:34]=[CH:33][C:32]=3[Br:39])[CH2:26][CH2:25]2)=[CH:18][CH:17]=1)=O)(C)(C)C>>[ClH:7].[NH2:15][C:16]1[CH:17]=[CH:18][C:19]([CH2:22][CH2:23][N:24]2[CH2:25][CH2:26][CH:27]([CH2:30][C:31]3[CH:36]=[C:35]([O:37][CH3:38])[CH:34]=[CH:33][C:32]=3[Br:39])[CH2:28][CH2:29]2)=[CH:20][CH:21]=1

Participants

3

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 22675352HCID 22675352, compound

Product 1

HCID 22675293HCID 22675293, compoundYield 93%

Procedure

To a 4N hydrogen chloride-1,4-dioxane solution (5 ml) was added 2-(4-tert-butoxycarbonylaminophenyl)ethyl-4-(2-bromo-5-methoxybenzyl)piperidine (580 mg, 1.15 mmol) in small portions at room temperature, and the reaction mixture was stirred as it was for 2 hours. After the solvent was distilled off under reduced pressure, the residue was suspended in ethyl acetate-diethyl ether, and the precipitate was collected by filtration and washed with diethyl ether to obtain the title compound (509 mg, 93%) as light-brown powder.

Workup

  1. distillationAfter the solvent was distilled off under reduced pressure
  2. filtrationthe precipitate was collected by filtration
  3. washwashed with diethyl ether

Sources & evidence

ORD record
ord-01e76faf712748bd92c9f1bd6fa242f1
Source dataset
uspto-grants-2004_09
Patent number
US06787560B2

Reaction notes

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