Hydrochloric Acid → HCID 13145491, compound

HRID 464003Notes

Reaction equation

HRID 464003 reaction equation
C(OCC)(=O)C.O.O.[Cl:9][C:10]1[CH:29]=[CH:28][C:13]([C:14]([NH:16][C:17]([CH2:24][CH2:25][C:26]#[N:27])([C:21]([O-:23])=[O:22])[C:18]([O-:20])=[O:19])=[O:15])=[CH:12][CH:11]=1.[Na+].[Na+].Cl>O>[Cl:9][C:10]1[CH:11]=[CH:12][C:13]([C:14]([NH:16][C:17]([CH2:24][CH2:25][C:26]#[N:27])([C:21]([OH:23])=[O:22])[C:18]([OH:20])=[O:19])=[O:15])=[CH:28][CH:29]=1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 20263534HCID 20263534, compound

Product 1

HCID 13145491HCID 13145491, compoundYield 100.6%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

Fifty milliliters of ethyl acetate were added to a solution of 4.0 g of disodium 2-(p-chlorobenzoylamino)-2-(2-cyanoethyl)malonate dihydrate in water (50 ml), and the resulting solution was adjusted to pH 2.0 by adding 1N hydrochloric acid at 0°-5° C. The organic layer was separated off and dried over magnesium sulphate. The solvent was distilled off and the resulting residue was recrystallized from diethyl ether, to give 3.2 g of the desired acid (b) as a colourless powder melting at 103°-105° C. (with decomposition).

Workup

  1. customThe organic layer was separated off
  2. dry with materialdried over magnesium sulphate
  3. distillationThe solvent was distilled off
  4. customthe resulting residue was recrystallized from diethyl ether

Sources & evidence

ORD record
ord-4f1bd30150ec49138272d81c40d2ec04
Source dataset
uspto-grants-1985_10
Patent number
US04545942

Reaction notes

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