Hydroxylamine → HCID 72806160, 화합물

HRID 354239

반응식

HRID 354239 반응식
[F:1][C:2]1[CH:3]=[C:4]([C:8](=O)[CH2:9][C:10]2[CH:15]=[CH:14][C:13]([C:16]([F:19])([F:18])[F:17])=[CH:12][N:11]=2)[CH:5]=[CH:6][CH:7]=1.[NH2:21][OH:22].[OH-].[Na+].CO>O>[F:1][C:2]1[CH:3]=[C:4]([C:8](=[N:21][OH:22])[CH2:9][C:10]2[CH:15]=[CH:14][C:13]([C:16]([F:19])([F:18])[F:17])=[CH:12][N:11]=2)[CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 4

HCID 787HydroxylamineHCID 887MethanolHCID 14798Sodium HydroxideHCID 129887451-(3-Fluorophenyl)-2-(5-trifluoromethyl-2-pyridinyl)ethanone

생성물 1

HCID 72806160HCID 72806160, 화합물수율 91%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
70 °C

실험 절차

A reaction vessel was charged with 1-(3-fluorophenyl)-2-(5-trifluoromethyl-2-pyridinyl)ethanone (2 g, 7 mmol), hydroxylamine (2.2 g, 32 mmol), 10% NaOH aqueous solution (11 ml, 27 mmol) and methanol (24 ml). The reaction mixture was heated to 70° C. and stirred at 70° C. for 3 hrs. It was then cooled to room temperature and water (12 ml) was added. The mixture was stirred at 0° C. for 1 hr. The solids were collected on a filter, washed with water, and dried under vacuum at 50° C. overnight to provide 1.9 g (91%) of the title compound as a solid with purity 99% AUC by HPLC (Phenomenex Luna 3μ cyano, 100 mm×4.6 mm. Flow rate: 1 ml/min. UV detection: 220 nm. Eluent: 75% A, 25% B. A: 80/20/0.05 water/acetonitrile/TFA. B: 20/80/0.05 water/acetonitrile/TFA).

후처리

  1. temperatureIt was then cooled to room temperature
  2. stirringThe mixture was stirred at 0° C. for 1 hr
  3. customThe solids were collected on a filter
  4. washwashed with water
  5. customdried under vacuum at 50° C. overnight

출처 및 근거

ORD 기록
ord-a68f2c02654c40518672bc02054c98b6
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06756498B2

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