Triethylamine → N-(4-bromo-3-fluorophenyl)pyridine-2-carboxamide

HRID 2080658

반응식

HRID 2080658 반응식
C(N(CC)CC)C.Cl.[N:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[C:15](Cl)=[O:16].[Br:18][C:19]1[CH:25]=[CH:24][C:22]([NH2:23])=[CH:21][C:20]=1[F:26]>C(Cl)(Cl)Cl>[Br:18][C:19]1[CH:25]=[CH:24][C:22]([NH:23][C:15]([C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][N:9]=2)=[O:16])=[CH:21][C:20]=1[F:26]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 135033Picolinoyl Chloride HydrochlorideHCID 8218484-Bromo-3-fluoroaniline

생성물 1

HCID 23145244N-(4-bromo-3-fluorophenyl)pyridine-2-carboxamide수율 92.7%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

2.9 ml of triethylamine and 1.87 g of picolinic acid chloride hydrochloride were added to a chloroform (30 ml) solution of 1 g of 4-bromo-3-fluoroaniline, and stirred at room temperature for 4 hours. The reaction liquid was diluted with chloroform, washed with aqueous saturated sodium bicarbonate solution and saturated saline water, and dried with anhydrous magnesium sulfate. The solvent was evaporated away, and the residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=4/1) to obtain 1.44 g of the entitled compound as a pale yellow crystal.

후처리

  1. customThe reaction liquid
  2. washwashed with aqueous saturated sodium bicarbonate solution and saturated saline water
  3. dry with materialdried with anhydrous magnesium sulfate
  4. customThe solvent was evaporated away
  5. customthe residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=4/1)

출처 및 근거

ORD 기록
ord-d0c1e3ecd2c34458b553a72b4096c6c1
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07932394B2

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