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Potassium Carbonate → HCID 20522427、化合物

HRID 223422
ノート
印刷プレビュー

反応式

HRID 223422 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[OH:9].Br[CH:11]([CH3:17])[C:12]([N:14]([CH3:16])[CH3:15])=[O:13].C(=O)([O-])[O-].[K+].[K+]>C(C(C)=O)C(C)C>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[O:9][CH:11]([CH3:17])[C:12]([N:14]([CH3:16])[CH3:15])=[O:13]
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 11430Potassium CarbonateHCID 113673482-Bromo-N,N-dimethylpropanamideHCID 132842722-Bromo-5-chlorophenol

生成物 1

HCID 20522427HCID 20522427、化合物

試薬・触媒・溶媒 1

HCID 7909Methyl Isobutyl Ketone溶媒

実験手順

2-Bromo-5-chlorophenol (8 g), 2-bromo-N,N-dimethylpropionamide (6.66 g) and anhydrous potassium carbonate (2.6 g) in methyl iso-butyl ketone (100 ml) were refluxed with stirring overnight. The mixture was cooled to 50° and washed with 5% sodium hydroxide (2×20 ml) and then water (2×50 ml). The organic solution was dried and evaporated under reduced pressure to yield a pale red oil, which solidified on cooling. Recrystallisation from 50% aqueous ethanol gave the title compound, m.p. 76°-77°. Compounds 2, 9, 10 to 13, 17 and 21 were made by a similar procedure.

後処理

  1. temperatureThe mixture was cooled to 50°
  2. washwashed with 5% sodium hydroxide (2×20 ml)
  3. customThe organic solution was dried
  4. customevaporated under reduced pressure
  5. customto yield a pale red oil, which
  6. temperatureon cooling
  7. customRecrystallisation from 50% aqueous ethanol

出典と根拠

ORDレコード
ord-ad3a008e04e24562b6d7371dc02fdf10
出典データセット
uspto-grants-1982_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04354034

反応ノート

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