Ethylene Glycol → 3-(1,3-Dioxolan-2-yl)-2-fluoro-4-iodopyridine

HRID 47356노트

반응식

HRID 47356 반응식
[F:1][C:2]1[C:7]([CH:8]=[O:9])=[C:6]([I:10])[CH:5]=[CH:4][N:3]=1.[CH2:11](O)[CH2:12][OH:13].C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1>[O:9]1[CH2:11][CH2:12][O:13][CH:8]1[C:7]1[C:2]([F:1])=[N:3][CH:4]=[CH:5][C:6]=1[I:10]

참가 물질

5

반응물 3

HCID 174Ethylene GlycolHCID 6101p-Toluenesulfonic acidHCID 99923282-Fluoro-4-iodopyridine-3-carbaldehyde

생성물 1

HCID 227449983-(1,3-Dioxolan-2-yl)-2-fluoro-4-iodopyridine

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

In a three-necked flask equipped with a Dean Stark apparatus, a mixture of 5.1 g (20.3 mmol) of 2-fluoro-4-iodo-3-pyridinecarbaldehyde, 1.4 g (22.3 mmol) of ethane-1,2-diol, and 50 mg of para-toluenesulphonic acid in 100 ml of toluene is heated at reflux. When the theoretical amount of water has been collected, the reaction mixture is cooled to room temperature, washed with a saturated sodium hydrogen carbonate solution and dried over magnesium sulphate. The expected product is obtained by concentration.

후처리

  1. customIn a three-necked flask equipped with a Dean Stark apparatus
  2. temperatureis heated
  3. temperatureat reflux
  4. customWhen the theoretical amount of water has been collected
  5. washwashed with a saturated sodium hydrogen carbonate solution
  6. dry with materialdried over magnesium sulphate

출처 및 근거

ORD 기록
ord-3b63d8bc500e47359ae59cf766c7223d
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06699876B2

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