Triethylamine → HCID 10179991, compound

HRID 411275Notes

Reaction equation

HRID 411275 reaction equation
[CH3:1][CH:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.C(N(CC)CC)C.[Cl:15][C:16]1[C:21]([C:22]2[CH:27]=[C:26]([F:28])[CH:25]=[CH:24][C:23]=2[C:29]([F:32])([F:31])[F:30])=[C:20](Cl)[N:19]2[N:34]=[CH:35][N:36]=[C:18]2[N:17]=1>ClCCl>[Cl:15][C:16]1[C:21]([C:22]2[CH:27]=[C:26]([F:28])[CH:25]=[CH:24][C:23]=2[C:29]([F:32])([F:30])[F:31])=[C:20]([N:5]2[CH2:6][CH2:7][CH:2]([CH3:1])[CH2:3][CH2:4]2)[N:19]2[N:34]=[CH:35][N:36]=[C:18]2[N:17]=1

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 693814-MethylpiperidineHCID 9924572HCID 9924572, compound

Product 1

HCID 10179991HCID 10179991, compoundYield 57.9%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Procedure

A mixture of 4-methylpiperidine(1.42 mmoles), triethylamine (1.42 mmoles) and dichloromethane (10 ml) is added to a mixture of 5,7-dichloro-6-(5-fluoro-2-trifluoromethyl-phenyl)-[1,2,4]-triazolo[1,5-α]pyrimidine (1.42 mmol) and dichloromethane (30 ml) under stirring. The reaction mixture is stirred 48 hours at room temperature and subsequently washed with dilute hydrochloric acid (5%). The organic layer is separated, dried with anhydrous sodium sulfate and filtered. The filtrate is evaporated under reduced pressure to yield 0.34 g of white crystals having a melting point of 149° C.

Workup

  1. stirringThe reaction mixture is stirred 48 hours at room temperature
  2. washsubsequently washed with dilute hydrochloric acid (5%)
  3. customThe organic layer is separated
  4. dry with materialdried with anhydrous sodium sulfate
  5. filtrationfiltered
  6. customThe filtrate is evaporated under reduced pressure

Sources & evidence

ORD record
ord-e83d46c538e04d439552fc18541262a5
Source dataset
uspto-grants-2003_05
Patent number
US06559151B2

Reaction notes

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