Pyridine → N-(1,3-dibromodibenzo[b,d]furan-4-yl)acetamide

HRID 1750917ノート

反応式

HRID 1750917 の反応式
[Br:1][C:2]1[C:10]2[C:9]3[CH:11]=[CH:12][CH:13]=[CH:14][C:8]=3[O:7][C:6]=2[C:5]([NH2:15])=[C:4]([Br:16])[CH:3]=1.N1C=CC=CC=1.[C:23](Cl)(=[O:25])[CH3:24]>ClCCl>[Br:1][C:2]1[C:10]2[C:9]3[CH:11]=[CH:12][CH:13]=[CH:14][C:8]=3[O:7][C:6]=2[C:5]([NH:15][C:23](=[O:25])[CH3:24])=[C:4]([Br:16])[CH:3]=1

参加物

5

反応物 3

HCID 1049PyridineHCID 6367Acetyl chlorideHCID 584010661,3-Dibromodibenzo[b,d]furan-4-amine

生成物 1

HCID 58400857N-(1,3-dibromodibenzo[b,d]furan-4-yl)acetamide収率 70.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

In a 2 L round-bottomed flask, 1,3-dibromodibenzo[b,d]furan-4-amine (76 g, 223 mmol) in dichloromethane (800 mL) and pyridine (180 mL, 2229 mmol) were cooled by ice bath. Acetyl chloride (31.7 mL, 446 mmol) was added dropwise while stirring. Then the ice bath was removed. The reaction was stirred at room temperature for 1 h. The residue was collected by filtration and washed by water and dichloromethane to give N-(1,3-dibromodibenzo[b,d]furan-4-yl)acetamide (60 g, 70.3% yield) as brown solid.

後処理

  1. customThen the ice bath was removed
  2. stirringThe reaction was stirred at room temperature for 1 h
  3. filtrationThe residue was collected by filtration
  4. washwashed by water and dichloromethane

出典と根拠

ORDレコード
ord-61240f818c4c40c08651ddf6cc23109d
出典データセット
uspto-grants-2015_10
特許番号
US09156870B2

反応ノート

読み込み中…