Lithium Hydroxide → HCID 19391289, compound

HRID 1757005Notes

Reaction equation

HRID 1757005 reaction equation
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:14][CH2:13][N:12]([CH2:15][C:16]([O:18]C)=[O:17])[CH2:11][CH2:10]2)=[CH:5][CH:4]=1)#[N:2].[OH-].[Li+].[Cl-].[NH4+]>O1CCCC1>[C:16]([CH2:15][N:12]1[CH2:13][CH2:14][N:9]([C:6]2[CH:7]=[CH:8][C:3]([C:1]#[N:2])=[CH:4][CH:5]=2)[CH2:10][CH2:11]1)([OH:18])=[O:17]

Participants

5

Reactant 3

HCID 3939Lithium HydroxideHCID 25517Ammonium ChlorideHCID 19391362Methyl 4-(4-cyanophenyl)-1-piperazineacetate

Product 1

HCID 19391289HCID 19391289, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

To 3 g of 1-(4-cyanophenyl)-4-(methoxycarbonylmethyl)-piperazine in 46 ml of tetrahydrofuran 58 ml of a 1 molar aqueous lithium hydroxide solution are added, at ambient temperature and with stirring, and the reaction solution is left to stand for 3 hours at ambient temperature. Then 3.2 g of ammonium chloride are added and the tetrahydrofuran is distilled off under reduced pressure. The precipitate is suction filtered, washed with water and dried. Yield: 2.2 g (77% of theory), Melting point: over 300° C. Rf value: 0.18 (silica gel; methylene chloride/methanol=9:1)

Workup

  1. waitthe reaction solution is left
  2. distillationthe tetrahydrofuran is distilled off under reduced pressure
  3. filtrationfiltered
  4. washwashed with water
  5. customdried
  6. customover 300° C

Sources & evidence

ORD record
ord-758e6b77e4b14c9992422da40c43bc0e
Source dataset
uspto-grants-1995_08
Patent number
US05442064

Reaction notes

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