Hydroxylamine, O-ethyl- → HCID 136017205, compound

HRID 2164363Notes

Reaction equation

HRID 2164363 reaction equation
[CH2:1]([NH:3][C:4](=[S:24])[NH:5][C:6]1[CH:11]=[CH:10][C:9]([CH:12]2[CH2:17][C:16](=[O:18])[C:15]([C:19](=O)[CH2:20][CH3:21])=[C:14]([OH:23])[CH2:13]2)=[CH:8][CH:7]=1)[CH3:2].[CH2:25]([O:27][NH2:28])[CH3:26]>C(Cl)(Cl)Cl>[CH2:25]([O:27][N:28]=[C:19]([C:15]1[C:16](=[O:18])[CH2:17][CH:12]([C:9]2[CH:8]=[CH:7][C:6]([NH:5][C:4]([NH:3][CH2:1][CH3:2])=[S:24])=[CH:11][CH:10]=2)[CH2:13][C:14]=1[OH:23])[CH2:20][CH3:21])[CH3:26]

Participants

4

Reactant 2

HCID 69357Hydroxylamine, O-ethyl-HCID 178465509HCID 178465509, compound

Product 1

HCID 136017205HCID 136017205, compoundYield 88.9%

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

Into 10 ml of chloroform was dissolved 1.4 g of 5-{4-[3-(ethyl)thioureido]phenyl}-3-hydroxy-2-propionyl-2-cyclohexen-1-one and to the solution was added 1.0 g of ethoxyamine. The mixture was kept for 15 hours at room temperature and the reacting mixture was washed with a dilute hydrochloric acid solution and water. The solution was dried with anhydrous magnesium sulfate and the chloroform was distilled off from it under reduced pressure and 1.4 g of the desired compound was obtained. It was in the form of colorless crystals having a decomposition point of 116°-118° C.

Workup

  1. washthe reacting mixture was washed with a dilute hydrochloric acid solution and water
  2. dry with materialThe solution was dried with anhydrous magnesium sulfate
  3. distillationthe chloroform was distilled off from it under reduced pressure

Sources & evidence

ORD record
ord-47597b6b219548cda2eb5fdcbacec4ac
Source dataset
uspto-grants-1985_03
Patent number
US04504305

Reaction notes

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