Hydrochloric Acid → 2,4-Dibromo-N-(4-bromophenyl)butanamide

HRID 715923

反応式

HRID 715923 の反応式
[Br:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[CH:4][CH:3]=1.[Br:9][CH:10]([CH2:14][CH2:15][Br:16])[C:11](Cl)=[O:12].Cl>ClCCl.C(N(CC)CC)C>[Br:9][CH:10]([CH2:14][CH2:15][Br:16])[C:11]([NH:6][C:5]1[CH:7]=[CH:8][C:2]([Br:1])=[CH:3][CH:4]=1)=[O:12]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 78074-BromoanilineHCID 44131432,4-Dibromobutyryl chloride

生成物 1

HCID 1178748012,4-Dibromo-N-(4-bromophenyl)butanamide

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒2 回HCID 8471Triethylamine溶媒

実験手順

To a solution of 4-bromoaniline (1.73 g) in dichloromethane (40 ml), triethylamine (2.8 ml) and a solution of 2,4-dibromobutyryl chloride (3.2 g) in dichloromethane (10 ml) were added under ice cooling, and the mixture was stirred at room temperature for 5 hours. After addition of 1 N hydrochloric acid to the reaction solution, the mixture was separated into two layers. The aqueous layer was subjected to extraction with chloroform. The organic layers were combined, washed with a saturated aqueous solution of sodium bicarbonate and saturated saline in this order and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain a crude product of the title compound, which was used in the next reaction without being purified.

後処理

  1. customthe mixture was separated into two layers
  2. extractionThe aqueous layer was subjected to extraction with chloroform
  3. washwashed with a saturated aqueous solution of sodium bicarbonate and saturated saline in this order
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-8338ee55c374481c9bb6df8e9bdb033b
出典データセット
uspto-grants-2015_11
特許番号
US09187489B2

関連ノート

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