Water → HCID 18321661, compound

HRID 1698779Notes

Reaction equation

HRID 1698779 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]CC)=[O:17])[C:11](=[O:21])[CH2:10]2)=[CH:5][CH:4]=1)#[N:2].O1CCCC1.O.O.[OH-].[Li+]>CO>[C:1]([C:3]1[CH:4]=[CH:5][C:6]([N:9]2[CH2:14][CH2:13][N:12]([CH2:15][C:16]([OH:18])=[O:17])[C:11](=[O:21])[CH2:10]2)=[CH:7][CH:8]=1)#[N:2]

Participants

6

Reactant 4

HCID 962WaterHCID 8028TetrahydrofuranHCID 168937Lithium hydroxide, monohydrateHCID 18321655HCID 18321655, compound

Product 1

HCID 18321661HCID 18321661, compoundYield 100%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

Ethyl 2-[4-(4-cyanophenyl)-2-oxopiperazino]-acetate (20.7 g, 72 mmol) is dissolved in 80 ml of methanol, 80 ml of tetrahydrofuran and 100 ml of water, and lithium hydroxide monohydrate (4 g, 98 mmol) is then added. Stirring is continued for 20 minutes and the organic solvent is then removed under vacuum. About 100 ml of water are added to the suspension obtained and this mixture is acidified. The product is filtered off, rinsed with water and dried under vacuum at 50° C. to give 18.5 g of a beige-coloured powder.

Workup

  1. customthe organic solvent is then removed under vacuum
  2. additionAbout 100 ml of water are added to the suspension
  3. customobtained
  4. filtrationThe product is filtered off
  5. washrinsed with water
  6. customdried under vacuum at 50° C.

Sources & evidence

ORD record
ord-a1b02a92a7e34ccd9b22a276ebbb21eb
Source dataset
uspto-grants-2002_02
Patent number
US06344456B1

Reaction notes

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