Dichloromethane → HCID 20327288, compound

HRID 1863495Notes

Reaction equation

HRID 1863495 reaction equation
C([N:3]([C:9]1[CH:14]=[C:13]([C:15]#[N:16])[C:12]([Cl:17])=[C:11]([NH2:18])[C:10]=1[Cl:19])[C:4](=[O:8])[C:5]([O-:7])=[O:6])C.C(Cl)Cl.[OH-].[Na+].[Na]>O>[NH2:18][C:11]1[C:10]([Cl:19])=[C:9]([NH:3][C:4](=[O:8])[C:5]([OH:7])=[O:6])[CH:14]=[C:13]([C:15]#[N:16])[C:12]=1[Cl:17]

Participants

6

Reactant 4

HCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 5360545SodiumHCID 20391934HCID 20391934, compound

Product 1

HCID 20327288HCID 20327288, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

A solution of 2.97 g. (0.01 mole) of ethyl(3-amino-2,4-dichloro-5-cyanophenyl)oxamate in 100 ml. of methylene chloride is placed in a separatory funnel. There is added a solution of 8 ml. of 1 N sodium hydroxide diluted to 100 ml. with water. There is added an additional 300 ml. of water to dissolve the sodium salt that forms. The phases are separated and the aqueous layer acidified with glacial acetic acid. To the solution is then added 5 ml. of concentrated hydrochloric acid. The precipitate is removed by filtration.

Workup

  1. additionThere is added a solution of 8 ml
  2. additionThere is added an additional 300 ml
  3. customThe phases are separated
  4. additionTo the solution is then added 5 ml
  5. customThe precipitate is removed by filtration

Sources & evidence

ORD record
ord-394c217c17ed49f8927d66a0c1fd7d93
Source dataset
uspto-grants-1979_09
Patent number
US04169153

Reaction notes

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