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Benzyl 2-(3,5-dichloro-2,6-difluoropyridin-4-yl)acetate → 3,5-Dichloro-2,6-difluoro-4-pyridineacetic acid

HRID 426296
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HRID 426296 반응식
[Cl:1][C:2]1[C:3]([F:21])=[N:4][C:5]([F:20])=[C:6]([Cl:19])[C:7]=1[CH2:8][C:9]([O:11]CC1C=CC=CC=1)=[O:10]>[Pd].C(O)C>[Cl:19][C:6]1[C:5]([F:20])=[N:4][C:3]([F:21])=[C:2]([Cl:1])[C:7]=1[CH2:8][C:9]([OH:11])=[O:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 59184758Benzyl 2-(3,5-dichloro-2,6-difluoropyridin-4-yl)acetate

생성물 1

HCID 591847703,5-Dichloro-2,6-difluoro-4-pyridineacetic acid수율 93.3%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

Benzyl 2-(3,5-dichloro-2,6-difluoropyridin-4-yl)acetate (30.9 g, 93 mmol), anhydrous ethanol, and 10% palladium on carbon were placed into a 500 mL bottle. The mixture was then hydrogenated using Parr Hydrogenator under hydrogen atmosphere (20 psi) for 30 min. The reaction mixture was then filtered through celite pad and the pad was washed with ethanol. The filtrate was evaporated in vacuo and the residue was recrystallized from MC to afford 21 g (89%) of 2-(3,5-dichloro-2,6-difluoropyridin-4-yl)acetic acid as a white solid. m.p. 157-159° C. 1H NMR (200 MHz, CDCl3) δ 4.13 (2H, s).

후처리

  1. customfor 30 min
  2. filtrationThe reaction mixture was then filtered through celite pad
  3. washthe pad was washed with ethanol
  4. customThe filtrate was evaporated in vacuo
  5. customthe residue was recrystallized from MC

출처 및 근거

ORD 기록
ord-36ec8a70541d4d33a01a91cbe50dbf25
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08106064B2

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