Sodium Hydroxide → HCID 20263534, compound

HRID 464002Notes

Reaction equation

HRID 464002 reaction equation
[OH-:1].[Na+:2].[Cl:3][C:4]1[CH:27]=[CH:26][C:7]([C:8]([N:10](CCC#N)[CH:11]([C:17]([O:19]CC)=[O:18])[C:12]([O:14]CC)=[O:13])=[O:9])=[CH:6][CH:5]=1>CO>[OH2:9].[OH2:1].[Cl:3][C:4]1[CH:5]=[CH:6][C:7]([C:8]([NH:10][C:11]([CH2:6][CH2:7][C:8]#[N:10])([C:17]([O-:19])=[O:18])[C:12]([O-:14])=[O:13])=[O:9])=[CH:26][CH:27]=1.[Na+:2].[Na+:2]

Participants

4

Reactant 2

HCID 14798Sodium HydroxideHCID 20263543HCID 20263543, compound

Product 1

HCID 20263534HCID 20263534, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A 1N solution of sodium hydroxide (80 ml) was added dropwise to a solution of 7.3 g of diethyl N-(p-chlorobenzoyl)-2-(2-cyanoethyl)aminomalonate in methanol (60 ml) at 0°-5° C., and the resulting mixture was stirred at room temperature for 16 hours. The reaction mixture was then concentrated under reduced pressure to a volume of 80 ml, and 60 ml of ethanol were added to the concentrate. The precipitate was filtered off, washed with 50 ml of ethanol and dried for 16 hours in vacuo, to afford 6.0 g of the desired disodium salt (a) as a colourless powder melting at 254°-255° C. (with decomposition).

Workup

  1. concentrationThe reaction mixture was then concentrated under reduced pressure to a volume of 80 ml, and 60 ml of ethanol
  2. additionwere added to the concentrate
  3. filtrationThe precipitate was filtered off
  4. washwashed with 50 ml of ethanol
  5. customdried for 16 hours in vacuo

Sources & evidence

ORD record
ord-3162c679911d445e8d554706fe07d447
Source dataset
uspto-grants-1985_10
Patent number
US04545942

Reaction notes

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