Hydroxyamine hydrochloride → HCID 86607960, compound

HRID 1803829Notes

Reaction equation

HRID 1803829 reaction equation
[CH3:1][CH2:2][C@@H:3]([CH:28]([CH3:30])[CH3:29])[CH2:4][CH2:5][C@H:6]([C@@H:8]1[C@:25]2([CH3:26])[C@H:11]([C@H:12]3[C@H:22]([CH2:23][CH2:24]2)[C@:20]2([CH3:21])[C:15](=[CH:16][C:17](=O)[CH2:18][CH2:19]2)[CH2:14][CH2:13]3)[CH2:10][CH2:9]1)[CH3:7].Cl.[NH2:32][OH:33]>N1C=CC=CC=1>[CH3:1][CH2:2][C@@H:3]([CH:28]([CH3:30])[CH3:29])[CH2:4][CH2:5][C@H:6]([C@@H:8]1[C@:25]2([CH3:26])[C@H:11]([C@H:12]3[C@H:22]([CH2:23][CH2:24]2)[C@:20]2([CH3:21])[C:15](=[CH:16][C:17](=[N:32][OH:33])[CH2:18][CH2:19]2)[CH2:14][CH2:13]3)[CH2:10][CH2:9]1)[CH3:7]

Participants

4

Reactant 2

HCID 443297Hydroxyamine hydrochlorideHCID 5484202Stigmast-4-en-3-one

Product 1

HCID 86607960HCID 86607960, compoundYield 50%

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

100 mg of 4-stigmasta-ene-3-one (0.24 mmol) is solubilized in 10 ml of pyridine in a 50 ml flask, then 100 mg of hydroxylamine hydrochloride is added. Stirring is maintained for 24 hours at ambient temperature, and the solvent is evaporated off under reduced pressure. Water then ethyl acetate is added in order to carry out an extraction. Then the organic phase is washed with an acidified aqueous solution (HCl 1%). The ethyl acetate is evaporated off under reduced pressure. A white powder is obtained with a yield greater than 50%.

Workup

  1. customthe solvent is evaporated off under reduced pressure
  2. additionWater then ethyl acetate is added in order
  3. extractionan extraction
  4. washThen the organic phase is washed with an acidified aqueous solution (HCl 1%)
  5. customThe ethyl acetate is evaporated off under reduced pressure
  6. customA white powder is obtained with a yield greater than 50%

Sources & evidence

ORD record
ord-e02b15599aaa45c19db0803a296f39b4
Source dataset
uspto-grants-2013_01
Patent number
US08354395B2

Reaction notes

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