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Dimethylformamide → Ace-011

HRID 748623
ノート
印刷プレビュー

反応式

HRID 748623 の反応式
[C:1]([NH:4][C:5]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:6]=1[OH:14])(=[O:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+].CN(C)C=O.[CH2:26](Br)[CH3:27]>O>[C:1]([NH:4][C:5]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:6]=1[O:14][CH2:26][CH3:27])(=[O:3])[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 6332Ethyl Bromide2 回HCID 11430Potassium CarbonateHCID 3749260N-(2-Hydroxy-4-nitrophenyl)acetamide

生成物 1

HCID 2877953Ace-011収率 100%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

To 400 g of 2-acetamido-5-nitrophenol in a 12-L, 4-necked flask equipped with a reflux condenser, nitrogen inlet, thermocouple, addition funnel, and mechanical stirrer was added 790 g of potassium carbonate and 2.0 L of dimethylformamide. The mixture was stirred at 60° C. as 294 g of ethyl bromide was added over 30 minutes. After 1 hour, an additional 27 g of ethyl bromide was added and the mixture was stirred at 60° C. for another hour. The mixture was cooled to room temperature and poured into 4 L of water. After 30 minutes, the product was collected by filtration and washed with water and heptane. The product was dried in a vacuum oven at 60° C. to give 457 g of the title compound.

後処理

  1. additionthermocouple, addition funnel, and mechanical stirrer
  2. additionwas added over 30 minutes
  3. temperatureThe mixture was cooled to room temperature
  4. waitAfter 30 minutes
  5. filtrationthe product was collected by filtration
  6. washwashed with water and heptane
  7. customThe product was dried in a vacuum oven at 60° C.

出典と根拠

ORDレコード
ord-2b1b7385f7f6411ba627529b1292801d
出典データセット
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07399865B2

反応ノート

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