Hydrochloric Acid → HCID 69518243, compound

HRID 1831401Notes

Reaction equation

HRID 1831401 reaction equation
[NH:1]1[CH2:6][CH2:5][CH:4]([CH2:7][N:8]2[CH2:13][CH2:12][CH:11]([OH:14])[CH2:10][CH2:9]2)[CH2:3][CH2:2]1.Cl.Cl[C:17]([O:19][C:20]1[CH:25]=[CH:24][C:23]([O:26][C:27]2[CH:32]=[CH:31][C:30]([C:33]([F:36])([F:35])[F:34])=[CH:29][N:28]=2)=[CH:22][CH:21]=1)=[O:18]>ClCCl.CN(C)C=O.C(OCC)(=O)C>[F:35][C:33]([F:34])([F:36])[C:30]1[CH:31]=[CH:32][C:27]([O:26][C:23]2[CH:24]=[CH:25][C:20]([O:19][C:17]([N:1]3[CH2:2][CH2:3][CH:4]([CH2:7][N:8]4[CH2:13][CH2:12][CH:11]([OH:14])[CH2:10][CH2:9]4)[CH2:5][CH2:6]3)=[O:18])=[CH:21][CH:22]=2)=[N:28][CH:29]=1

Participants

7

Reactant 3

HCID 313Hydrochloric Acid2×HCID 220477624-(5-Trifluoromethylpyridin-2-yloxy)-phenyl chloroformateHCID 220479421-[(Piperidin-4-yl)methyl]piperidin-4-ol

Product 1

HCID 69518243HCID 69518243, compound

Reagents, catalysts & solvents 3

HCID 6228DimethylformamideSolventHCID 6344DichloromethaneSolventHCID 8857Ethyl AcetateSolvent

Procedure

The title product was prepared from 1-piperidin-4-ylmethyl-piperidine-4-ol (released form the correspondent hydrochloride by a standard procedure) and 4-(5-trifluoromethyl-pyridin-2-yloxy)-phenyl chloroformate, preparative HPLC (method C) (reaction performed in a mixture of dichloromethane and dimethylformamide). 1.7 M HCl in ethyl acetate was added to the pooled fractions containing the title product, and the fractions was evaporated to dryness (92%, white solid. HPLC-MS m/z=(M+1) 480.4, Rt: 2.38 min.

Workup

  1. customreaction
  2. customthe fractions was evaporated to dryness (92%, white solid

Sources & evidence

ORD record
ord-8222277e045e437ca6a8abc6f3aee764
Source dataset
uspto-grants-2006_06
Patent number
US07067517B2

Reaction notes

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