Water → 1-(3-chloro-2-pyridinyl)-4-iodo-1H-pyrrole-2-carbaldehyde

HRID 251980노트

반응식

HRID 251980 반응식
[Cl:1][C:2]1[C:3]([N:8]2[CH:12]=[CH:11][CH:10]=[C:9]2[CH:13]=[O:14])=[N:4][CH:5]=[CH:6][CH:7]=1.[I:15]N1C(=O)CCC1=O.O>CN(C)C=O>[Cl:1][C:2]1[C:3]([N:8]2[CH:12]=[C:11]([I:15])[CH:10]=[C:9]2[CH:13]=[O:14])=[N:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 120273N-IodosuccinimideHCID 587620783-chloro-2-(2-formyl-1H-pyrrol-1-yl)pyridine

생성물 1

HCID 577802671-(3-chloro-2-pyridinyl)-4-iodo-1H-pyrrole-2-carbaldehyde수율 40.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 5.0 g of 3-chloro-2-(2-formyl-1H-pyrrol-1-yl)pyridine in 50 ml of N,N-dimethylformamide was added 5.4 g of N-iodosuccinimide. The resulting mixture was stirred at room temperature for 1 day. Water was poured into the reaction mixture, and the mixture was extracted with ethyl acetate two times. The organic layers were combined, washed with an aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 3.2 g of 1-(3-chloro-2-pyridinyl)-4-iodo-1H-pyrrole -2-carbaldehyde of the formula:

후처리

  1. extractionthe mixture was extracted with ethyl acetate two times
  2. washwashed with an aqueous saturated sodium chloride solution
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-765b9601886547dc83e36589b8c503b0
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07867949B2

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