Hydroxyamine hydrochloride → HCID 136378651, 화합물

HRID 527525노트

반응식

HRID 527525 반응식
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]

참가 물질

6

반응물 3

HCID 443297Hydroxyamine hydrochloride2회HCID 116223911-(2,6-Dihydroxyphenyl)-propan-1-one2회HCID 23665404Sodium Acetate Trihydrate2회

생성물 1

HCID 136378651HCID 136378651, 화합물수율 96.3%

시약·촉매·용매 2

HCID 962Water용매HCID 19096565Water ethanol용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-e2ff545c5e2c4e4195ea386ccb893408
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09346790B2

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