5-Bromopyridine-2-carboxamide → HCID 58149557, 화합물

HRID 1920082노트

반응식

HRID 1920082 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([NH2:10])=[O:9])=[N:6][CH:7]=1.[OH:11][CH:12](O)[C:13]([C:15]1[C:24]2[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=2)[CH:18]=[CH:17][CH:16]=1)=[O:14]>O1CCOCC1>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([NH:10][CH:12]([OH:11])[C:13]([C:15]2[C:24]3[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=3)[CH:18]=[CH:17][CH:16]=2)=[O:14])=[O:9])=[N:6][CH:7]=1

참가 물질

4

반응물 2

HCID 7351515-Bromopyridine-2-carboxamideHCID 5684550216208-20-1

생성물 1

HCID 58149557HCID 58149557, 화합물수율 66%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
100 °C

실험 절차

A mixture of 5-bromopicolinamide 111 (0.588 g, 2.92 mmol) and 2,2-dihydroxy-1-(naphthalen-1-yl)ethanone 112 (1.20 g, 5.67 mmol) in dioxane (20 mL) were heated at 100° C. for 18 hours. The dioxane was removed under vacuum and the residue was dissolved in chloroform and methanol and concentrated onto silica gel. The material was purified by auto flash system (CH2Cl2 to 1% MeOH: CH2Cl2) to give 5-bromo-N-(1-hydroxy-2-(naphthalen-1-yl)-2-oxoethyl)picolinamide 113 as a tan solid (0.74 g, 66%).

후처리

  1. customThe dioxane was removed under vacuum
  2. dissolutionthe residue was dissolved in chloroform
  3. concentrationmethanol and concentrated onto silica gel
  4. customThe material was purified by auto flash system (CH2Cl2 to 1% MeOH: CH2Cl2)

출처 및 근거

ORD 기록
ord-1eeb2caaeeac4f419dd0e77c598cef4c
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08168795B2

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