Potassium Carbonate → HCID 68281537、化合物

HRID 2278592ノート

反応式

HRID 2278592 の反応式
Br[CH2:2][C:3]([CH3:5])=[CH2:4].C(=O)([O-])[O-].[K+].[K+].[H-].[Na+].[Br:14][C:15]1[C:20]([F:21])=[CH:19][CH:18]=[CH:17][C:16]=1[NH:22][C:23](=[O:25])[CH3:24]>C1(C)C=CC=CC=1.C(OCC)(=O)C.O>[Br:14][C:15]1[C:20]([F:21])=[CH:19][CH:18]=[CH:17][C:16]=1[N:22]([CH2:2][C:3]([CH3:5])=[CH2:4])[C:23](=[O:25])[CH3:24]

参加物

8

反応物 4

HCID 11430Potassium CarbonateHCID 24758Sodium hydrideHCID 3577853-Bromo-2-methyl-1-propeneHCID 68281659HCID 68281659、化合物

生成物 1

HCID 68281537HCID 68281537、化合物収率 102.7%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 1140Toluene溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
75 °C

実験手順

2 g of 3-bromo-2-methylpropene, 1.9 g of potassium carbonate and 570 mg of sodium hydride (dispersion in oil at 60%) are added to a solution of 3 g of N-(2-bromo-3-fluorophenyl)acetamide in 25 ml of toluene. The reaction mixture is placed under an argon atmosphere and heated at 75° C. for 16 hours. The reaction mixture is treated with a mixture of water and ethyl acetate, and the organic phase is then washed with water and a saturated sodium chloride solution, dried over magnesium sulfate, filtered, and concentrated under reduced pressure, so as to give 3.8 g of N-(2-bromo-3-fluorophenyl)-N-(2-methylallyl)acetamide.

後処理

  1. washthe organic phase is then washed with water
  2. dry with materiala saturated sodium chloride solution, dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-6659366b4f4c4fb096465c7cad24912a
出典データセット
uspto-grants-2015_09
特許番号
US09133168B2

反応ノート

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