Phenyltrimethylammonium bromide dibromide → HCID 118071642、化合物

HRID 56005ノート

反応式

HRID 56005 の反応式
[Cl:1][C:2]1[C:3]([C:10](=[O:12])[CH3:11])=[N:4][CH:5]=[C:6]([O:8][CH3:9])[CH:7]=1.[Br-:13].[Br-].[Br-].C[N+](C)(C)C1C=CC=CC=1.C[N+](C1C=CC=CC=1)(C)C.C[N+](C1C=CC=CC=1)(C)C>O1CCCC1>[Br:13][CH2:11][C:10]([C:3]1[C:2]([Cl:1])=[CH:7][C:6]([O:8][CH3:9])=[CH:5][N:4]=1)=[O:12]

参加物

4

反応物 2

HCID 17977687Phenyltrimethylammonium bromide dibromideHCID 838765981-(3-Chloro-5-methoxypyridin-2-yl)ethanone

生成物 1

HCID 118071642HCID 118071642、化合物収率 76.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To 0.90 g of 1-(3-chloro-5-methoxypyridin-2-yl)ethanone in 10 ml of tetrahydrofuran, 1.82 g of trimethylphenylammonium tribromide was added, and the mixture was stirred at room temperature for 16 hours. After completion of the reaction, the precipitated solid was filtered off, and the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography using ethyl acetate-hexane (with a gradient of from 1:9 to 3:7) as the eluent to obtain 0.57 g of the desired product as pale yellow crystals.

後処理

  1. customAfter completion of the reaction
  2. filtrationthe precipitated solid was filtered off
  3. customthe solvent was evaporated under reduced pressure
  4. customThe resulting residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-41bd32319c9141c3a2e89490c2af54d8
出典データセット
uspto-grants-2016_09
特許番号
US09434684B2

反応ノート

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