Acetic Acid → HCID 20537580, compound

HRID 1155672Notes

Reaction equation

HRID 1155672 reaction equation
C(OC([NH:11][CH:12]1[CH2:16][C:15](=[O:17])[N:14]([C:18]2[CH:23]=[C:22]([Cl:24])[CH:21]=[C:20]([Cl:25])[CH:19]=2)[C:13]1=[O:26])=O)C1C=CC=CC=1.C(O)(=O)C.[BrH:31]>C(OCC)C>[BrH:31].[NH2:11][CH:12]1[CH2:16][C:15](=[O:17])[N:14]([C:18]2[CH:19]=[C:20]([Cl:25])[CH:21]=[C:22]([Cl:24])[CH:23]=2)[C:13]1=[O:26]

Participants

5

Reactant 3

HCID 176Acetic AcidHCID 260Hydrogen BromideHCID 20537575HCID 20537575, compound

Product 1

HCID 20537580HCID 20537580, compound

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

85 g of 3-(N-benzyloxycarbonylamino)-1-(3,5-dichlorophenyl)pyrrolidine-2,5-dione are mixed with 200 ml of a solution of glacial acetic acid which is saturated with hydrobromic acid, and the mixture is then stirred for 11/2 hours at room temperature. Then 1 liter of diethyl ether is added and the precipitated crystals are rapidly collected by filtration, washed with diethyl ether and dried over potassium hydroxide in vacuo. The hydrobromide is obtained in the form of colourless crystals which melt at 278°-280° C. with decomposition.

Workup

  1. filtrationthe precipitated crystals are rapidly collected by filtration
  2. washwashed with diethyl ether
  3. dry with materialdried over potassium hydroxide in vacuo

Sources & evidence

ORD record
ord-c472243b1c36446bb89a719b74b896b3
Source dataset
uspto-grants-1982_06
Patent number
US04332816

Reaction notes

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