Ethanol → 6-Nitro-4-chromanone Oxime

HRID 1764117

반응식

HRID 1764117 반응식
Cl.[NH2:2][OH:3].[OH-].[Na+].[N+:6]([C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[O:15][CH2:14][CH2:13][C:12]2=O)([O-:8])=[O:7].C(O)C>O>[N+:6]([C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[O:15][CH2:14][CH2:13][C:12]2=[N:2][OH:3])([O-:8])=[O:7]

참가 물질

6

반응물 4

HCID 702EthanolHCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 52288316-nitro-3,4-dihydro-2H-1-benzopyran-4-one

생성물 1

HCID 859699586-Nitro-4-chromanone Oxime

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of 79 g (1.14 mole) of hydroxylamine hydrochloride in 770 ml of H2O, contained in a 2 l. Erlenmeyer flask, was treated with 619 ml of 10% NaOH, 150 g (0.78 mole) of 6-nitro-4-chromanone and enough ethanol (750 ml) to produce a solution at the boiling point. The reaction mixture was boiled for 25 min., cooled to 50° over 2 hrs., and filtered. The filtrate was refrigerated overnight and filtered. The tan crystalline solid was washed with 200 ml of ethanol and dried, m.p. 173°-178°. Yield: 60 g (37%).

후처리

  1. customto produce a solution at the boiling point
  2. temperaturecooled to 50° over 2 hrs
  3. filtration, and filtered
  4. waitThe filtrate was refrigerated overnight
  5. filtrationfiltered
  6. washThe tan crystalline solid was washed with 200 ml of ethanol
  7. customdried

출처 및 근거

ORD 기록
ord-d64b3536d9a641eaa5934ddf2e7e49a1
출처 데이터셋
uspto-grants-1978_09
특허 번호
US04115405

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