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Pyridine → 2-bromo-N-(4-(trifluoromethoxy)phenyl)propanamide

HRID 1655552
ノート
印刷プレビュー

反応式

HRID 1655552 の反応式
[Br:1][CH:2]([CH3:6])[C:3](Cl)=[O:4].Cl.[F:8][C:9]([F:19])([F:18])[O:10][C:11]1[CH:17]=[CH:16][C:14]([NH2:15])=[CH:13][CH:12]=1.N1C=CC=CC=1>C(Cl)Cl>[Br:1][CH:2]([CH3:6])[C:3]([NH:15][C:14]1[CH:16]=[CH:17][C:11]([O:10][C:9]([F:8])([F:18])[F:19])=[CH:12][CH:13]=1)=[O:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1049PyridineHCID 979802-Bromopropanoyl chlorideHCID 27810604-(trifluoromethoxy)aniline Hydrochloride

生成物 1

HCID 197926812-bromo-N-(4-(trifluoromethoxy)phenyl)propanamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 4.02 g (23.4 mmol) of 2-bromopropionyl chloride in 10 ml of methylene chloride was added to an ice-cooled solution of 5.0 g (23.4 mmol) of 4-(trifluoromethoxy)aniline hydrochloride, 4.65 g (59 mmol) of pyridine and 30 ml of methylene chloride. The mixture was stirred at ambient temperature for a period of 2.5 hours and then washed with two portions of dilute aqueous HCl and two portions of saturated aqueous sodium bicarbonate, dried over MgSO4, treated with charcoal, filtered and the filtrates evaporated to dryness. The residue was recrystallized from methylcyclohexane to give 5.43 g 74 percent of theoretical) of the above-named product as colorless crystals, m.p. 111°-112° C.

後処理

  1. washwashed with two portions of dilute aqueous HCl and two portions of saturated aqueous sodium bicarbonate
  2. dry with materialdried over MgSO4
  3. additiontreated with charcoal
  4. filtrationfiltered
  5. customthe filtrates evaporated to dryness
  6. customThe residue was recrystallized from methylcyclohexane

出典と根拠

ORDレコード
ord-dd9c798f3f424ef982fb3206e63b003d
出典データセット
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05250690

反応ノート

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