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

HRID 2080658

反応式

HRID 2080658 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-d0c1e3ecd2c34458b553a72b4096c6c1
出典データセット
uspto-grants-2011_04
特許番号
US07932394B2

関連ノート

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