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Iodine chloride → 7-Chloro-3-(2-chlorophenyl)-4-iodo-2,6-naphthyridine 2-oxide

HRID 468861
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HRID 468861 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:8]([C:11]#[C:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[Cl:19])=[CH:9][N:10]=1)[CH:5]=[N:6][OH:7].[I:20]Cl>C(#N)C.C(OCC)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]2[C:8]([C:11]([I:20])=[C:12]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[Cl:19])[N+:6]([O-:7])=[CH:5]2)=[CH:9][N:10]=1
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참가 물질

5

반응물 2

HCID 24640Iodine chlorideHCID 1364131892-Chloro-5-((2-chlorophenyl)ethynyl)isonicotinaldehyde oxime

생성물 1

HCID 866749537-Chloro-3-(2-chlorophenyl)-4-iodo-2,6-naphthyridine 2-oxide

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 8857Ethyl Acetate용매

실험 절차

To a slurry of 2-chloro-5-((2-chlorophenyl)ethynyl)isonicotinaldehyde oxime (850 mg, 2.9 mmol) in acetonitrile (8 mL) was added iodine monochloride (1.4 g, 8.8 mmol). The reaction mixture instantly became homogeneous and was stirred at room temperature. After 15 minutes the reaction mixture was diluted with ethyl acetate (100 mL) and washed with water (100 mL). The organic layer was separated, dried over sodium sulfate, filtered, and evaporated in vacuo to afford an orange residue that was used in the next step without further purification (1.2 g, 98%).

후처리

  1. washwashed with water (100 mL)
  2. customThe organic layer was separated
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated in vacuo
  6. customto afford an orange residue that
  7. customwas used in the next step without further purification (1.2 g, 98%)

출처 및 근거

ORD 기록
ord-3abd70d1455f4a8a8821edb2264c2e87
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08623889B2

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