Chloroform → HCID 22931003, compound

HRID 459872Notes

Reaction equation

HRID 459872 reaction equation
C(Cl)(Cl)[Cl:2].[CH3:5][O:6][C:7]1[CH:8]=[C:9]([C:15]2[N:20]=[C:19]([C:21]([N:23]3[CH2:28][CH2:27][N:26]([C:29]4[CH:50]=[CH:49][C:32]([O:33][CH2:34][CH2:35][N:36]5[CH2:41][CH2:40][N:39](C(OC(C)(C)C)=O)[CH2:38][CH2:37]5)=[CH:31][CH:30]=4)[CH2:25][CH2:24]3)=[O:22])[CH:18]=[CH:17][CH:16]=2)[CH:10]=[CH:11][C:12]=1[O:13][CH3:14].[ClH:51].C(OCC)(=O)C>C(O)C>[OH2:6].[ClH:2].[ClH:51].[ClH:2].[ClH:2].[CH3:5][O:6][C:7]1[CH:8]=[C:9]([C:15]2[N:20]=[C:19]([C:21]([N:23]3[CH2:24][CH2:25][N:26]([C:29]4[CH:50]=[CH:49][C:32]([O:33][CH2:34][CH2:35][N:36]5[CH2:37][CH2:38][NH:39][CH2:40][CH2:41]5)=[CH:31][CH:30]=4)[CH2:27][CH2:28]3)=[O:22])[CH:18]=[CH:17][CH:16]=2)[CH:10]=[CH:11][C:12]=1[O:13][CH3:14]

Participants

5

Reactant 3

HCID 6212Chloroform2×HCID 18444296HCID 18444296, compoundHCID 21866389Hydrogen chloride-ethyl acetate2×

Product 1

HCID 22931003HCID 22931003, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a chloroform (3 ml) solution of t-butyl 4-[2-(4-{4-[6-(3,4-dimethoxyphenyl)pyridine-2-carbonyl]piperazin-1-yl}phenoxy)ethyl]piperazine-1-carboxylate was added 0.427 ml of a 4M hydrogen chloride/ethyl acetate solution, followed by 2 days of stirring at room temperature. Further, 2 ml of chloroform and 1 ml of a 4M hydrogen chloride/ethyl acetate solution were added thereto, and the whole was stirred at room temperature overnight. Ethanol was added to the reaction mixture and crude crystals were collected by filtration and recrystallized from methanol to obtain 114 mg of 1-[6-(3,4-dimethoxyphenyl)pyridine-2-carbonyl]-4-[4-(2-piperazin-1-ylethoxy)phenyl]piperazine tetrahydrochloride hydrate as pale yellow crystals.

Workup

  1. stirringthe whole was stirred at room temperature overnight
  2. filtrationcrude crystals were collected by filtration
  3. customrecrystallized from methanol

Sources & evidence

ORD record
ord-d4a303687891438ebc29016d2cb05b59
Source dataset
uspto-grants-2007_03
Patent number
US07196080B2

Reaction notes

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