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Sodium Iodide → HCID 23206543, 화합물

HRID 1289424
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HRID 1289424 반응식
[F:1][C:2]([F:14])([F:13])[C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[N:9]=[CH:8][CH:7]=[CH:6]2.[Cl:15][C:16]([Cl:23])([Cl:22])[CH2:17][O:18][C:19](Cl)=[O:20].[CH2:24]([O:26][P:27]([O:31]CC)[O:28][CH2:29][CH3:30])[CH3:25].[I-].[Na+]>C(#N)C>[CH2:24]([O:26][P:27]([CH:8]1[CH:7]=[CH:6][C:5]2[C:10](=[CH:11][CH:12]=[C:3]([C:2]([F:1])([F:13])[F:14])[CH:4]=2)[N:9]1[C:19]([O:18][CH2:17][C:16]([Cl:23])([Cl:22])[Cl:15])=[O:20])(=[O:31])[O:28][CH2:29][CH3:30])[CH3:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 5238Sodium IodideHCID 31215Triethyl phosphiteHCID 870632,2,2-Trichloroethyl chloroformateHCID 126475676-(Trifluoromethyl)quinoline

생성물 1

HCID 23206543HCID 23206543, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

41.4 g of 6-trifluoromethylquinoline is introduced into 250 ml of acetonitrile at 0° C. 29 ml of chloroformic acid-2,2,2-trichloroethyl ester is rapidly instilled and the mixture is stirred for 30 minutes. 36.4 ml of triethylphosphite is instilled and 49.8 g of sodium iodide is added in portions. It is heated for 10 minutes to 50° C., the solution is concentrated by evaporation, mixed with 400 ml of water and extracted four times with 400 ml of ethyl acetate each. The crude product is purified by column chromatography and recrystallized from isopropyl ether.

후처리

  1. temperatureIt is heated for 10 minutes to 50° C.
  2. concentrationthe solution is concentrated by evaporation
  3. additionmixed with 400 ml of water
  4. extractionextracted four times with 400 ml of ethyl acetate each
  5. customThe crude product is purified by column chromatography
  6. customrecrystallized from isopropyl ether

출처 및 근거

ORD 기록
ord-234356a5b0f6420ba5dd3c2eea3f6b30
출처 데이터셋
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05750526

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