Hydroxyamine hydrochloride → 2-Chloro-5-((2-chlorophenyl)ethynyl)isonicotinaldehyde oxime

HRID 468850노트

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HRID 468850 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:7]([C:10]#[C:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[Cl:18])=[CH:8][N:9]=1)[CH:5]=O.C([O-])(=O)C.[Na+].Cl.[NH2:25][OH:26]>C(O)C.ClC(Cl)C.C(OCC)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([C:7]([C:10]#[C:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[Cl:18])=[CH:8][N:9]=1)[CH:5]=[N:25][OH:26]

참가 물질

7

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 866749492-Chloro-5-((2-chlorophenyl)ethynyl)isonicotinaldehyde

생성물 1

HCID 1364131892-Chloro-5-((2-chlorophenyl)ethynyl)isonicotinaldehyde oxime

시약·촉매·용매 3

HCID 702Ethanol용매HCID 63651,1-Dichloroethane용매HCID 8857Ethyl Acetate용매

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온도
50 °C

실험 절차

A mixture of 2-chloro-5-((2-chlorophenyl)ethynyl)isonicotinaldehyde (1.1 g, 4.0 mmol), sodium acetate (490 mg, 6 mmol), and hyroxylamine hydrochloride (415 mg, 6 mmol) in ethanol (23 mL) and dichloroethane (13 mL) was heated at 50° C. for 15 minutes. The cooled reaction mixture was evaporated in vacuo to afford a residue that was redissolved in ethyl acetate (150 mL) and washed with water (100 mL). The organic layer was separated, dried over sodium sulfate, filtered, and evaporated in vacuo to afford a white solid that was used in the next step without further purification.

후처리

  1. customThe cooled reaction mixture
  2. customwas evaporated in vacuo
  3. customto afford a residue that
  4. washwashed with water (100 mL)
  5. customThe organic layer was separated
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. customevaporated in vacuo
  9. customto afford a white solid that
  10. customwas used in the next step without further purification

출처 및 근거

ORD 기록
ord-150dddf07c774851bcb9841ae1f580ad
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08623889B2

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