Methanol → HCID 178510745, 화합물

HRID 250810노트

반응식

HRID 250810 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]#[N:10])=[CH:4][CH:3]=1.Cl.[NH2:12][OH:13].C(=O)(O)[O-].[Na+].CO.O>>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([NH:12][OH:13])=[NH:10])=[CH:4][CH:3]=1

참가 물질

6

반응물 5

HCID 887MethanolHCID 962WaterHCID 27914Benzeneacetonitrile, 4-bromo-HCID 443297Hydroxyamine hydrochlorideHCID 516892Sodium Bicarbonate

생성물 1

HCID 178510745HCID 178510745, 화합물수율 85.6%

실험 절차

4-Bromophenylacetonitrile (5.0 g, 25.5 mmol), hydroxylamine hydrochloride (3.9 g, 56.1 mmol), and sodium bicarbonate (5.1 g, 61.2 mmol) were dissolved in MeOH (250 mL, 6.2 mol) and water (40 mL, 2 mol). The mixture was heated at reflux overnight, cooled, and then concentrated to 50 mL. The residue was dissolved in DCM, washed with water and saturated aqueous NaCl, dried over MgSO4, filtered and concentrated to yield 2-(4-bromophenyl)-N-hydroxyacetamidine (5.0 g).

후처리

  1. temperatureThe mixture was heated
  2. temperatureat reflux overnight
  3. temperaturecooled
  4. concentrationconcentrated to 50 mL
  5. dissolutionThe residue was dissolved in DCM
  6. washwashed with water and saturated aqueous NaCl
  7. dry with materialdried over MgSO4
  8. filtrationfiltered
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-63cf39fc596644ecaac044ae2bd50df8
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07863309B2

반응 노트

불러오는 중…