Hydroxyamine hydrochloride → HCID 136378651、化合物

HRID 527525ノート

反応式

HRID 527525 の反応式
Cl.[NH2:2][OH:3].O.O.O.C([O-])(=O)C.[Na+].[OH:12][C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([OH:19])[C:14]=1[C:20](=O)[CH2:21][CH3:22]>CCO.O.O>[OH:12][C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([OH:19])[C:14]=1[C:20](=[N:2][OH:3])[CH2:21][CH3:22]

参加物

6

反応物 3

HCID 443297Hydroxyamine hydrochloride2 回HCID 116223911-(2,6-Dihydroxyphenyl)-propan-1-one2 回HCID 23665404Sodium Acetate Trihydrate2 回

生成物 1

HCID 136378651HCID 136378651、化合物収率 96.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 19096565Water ethanol溶媒2 回

実験手順

A solution of hydroxylamine hydrochloride (510 mg, 7.3 mmol) and sodium acetate trihydrate (629 mg, 4.6 mmol) dissolved in 20 ml of a mixture EtOH/H2O (7/3) was added to a solution of 1-(2,6-dihydroxyphenyl)-1-propanone (Intermediate 28, 1.0 g) in 15 ml of a mixture EtOH/H2O (7/3). After refluxing and stirring under N2 overnight, additional hydroxylamine hydrochloride (510 mg, 7.3 mmol) and sodium acetate trihydrate (629 mg, 4.6 mmol) dissolved in 4.5 mL of water were added. The reaction mixture was heated at reflux an additional 3 hours. After cooling down to room temperature, the volatiles were removed. Then water was added and reaction mixture was extracted with ethyl acetate. The gathered organic layers were dried over sodium sulphate, filtered and evaporated to afford the title compound (1.05 g).

後処理

  1. temperatureAfter refluxing
  2. additionwere added
  3. temperatureThe reaction mixture was heated
  4. temperatureat reflux an additional 3 hours
  5. customthe volatiles were removed
  6. additionThen water was added
  7. customreaction mixture
  8. extractionwas extracted with ethyl acetate
  9. dry with materialThe gathered organic layers were dried over sodium sulphate
  10. filtrationfiltered
  11. customevaporated

出典と根拠

ORDレコード
ord-e2ff545c5e2c4e4195ea386ccb893408
出典データセット
uspto-grants-2016_05
特許番号
US09346790B2

反応ノート

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