Phenyltrimethylammonium bromide dibromide → HCID 118071642, 화합물

HRID 56005노트

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HRID 56005 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 118071642HCID 118071642, 화합물수율 76.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-41bd32319c9141c3a2e89490c2af54d8
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09434684B2

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