Hydroxyamine hydrochloride → 3-Fluoro-2-trifluoromethyl-pyridine-4-carbaldehyde oxime

HRID 1527468노트

반응식

HRID 1527468 반응식
[F:1][C:2]1[C:3]([C:10]([F:13])([F:12])[F:11])=[N:4][CH:5]=[CH:6][C:7]=1[CH:8]=O.Cl.[NH2:15][OH:16].C([O-])(=O)C.[NH4+]>CO.O>[F:1][C:2]1[C:3]([C:10]([F:13])([F:12])[F:11])=[N:4][CH:5]=[CH:6][C:7]=1[CH:8]=[N:15][OH:16]

참가 물질

6

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 517165Ammonium AcetateHCID 866738643-Fluoro-2-(trifluoromethyl)pyridine-4-carbaldehyde

생성물 1

HCID 1363523253-Fluoro-2-trifluoromethyl-pyridine-4-carbaldehyde oxime

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

To a solution of 3-fluoro-2-trifluoromethyl-pyridine-4-carbaldehyde (0.495 g, 2.05 mmol) in MeOH (17.6 mL) and water (2.9 mL) were added hydroxylamine hydrochloride (0.214 g, 3.08 mmol) and ammonium acetate (0.474 g, 6.15 mmol), and the resulting mixture was stirred at RT overnight. Volatile were removed in vacuo, and the residue was suspended in CH2Cl2/MeOH 9:1. The precipitate was filtered off, washed with CH2Cl2 and dried to afford the title compound as a white solid. MS (LC/MS): 209.0 [M+H]+; tR (HPLC conditions c): 4.28 min.

후처리

  1. customVolatile were removed in vacuo
  2. filtrationThe precipitate was filtered off
  3. washwashed with CH2Cl2
  4. customdried

출처 및 근거

ORD 기록
ord-423f296eef0f41c09ce34e77d16bcefb
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09085555B2

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