Hydrogen Peroxide → 9-Ethyl-3-iodocarbazole

HRID 1291975ノート

反応式

HRID 1291975 の反応式
[CH2:1]([N:3]1[C:15]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[C:9]2[C:4]1=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH3:2].[I:16]I.OO.S(=O)(=O)(O)O>O.C(O)(=O)C.O>[I:16][C:7]1[CH:6]=[CH:5][C:4]2[N:3]([CH2:1][CH3:2])[C:15]3[C:10]([C:9]=2[CH:8]=1)=[CH:11][CH:12]=[CH:13][CH:14]=3

参加物

7

反応物 4

HCID 784Hydrogen PeroxideHCID 807IodineHCID 1118Sulfuric AcidHCID 6836N-ethyl carbazole

生成物 1

HCID 40733629-Ethyl-3-iodocarbazole収率 126.9%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 21899381Acetic acid--water (1/1)溶媒

反応条件

温度
60 °C

実験手順

Into 5.0 g (25.6 mmol) of 9-ethylcarbazole, 40 ml of a 9:1 acetic acid-water mixture, 3.3 g (13.0 mmol) of iodine, 2.5 g of a 30% hydrogen peroxide solution, and 1.8 g of 97% sulfuric acid were added, and the mixture was stirred at 60° C for 2 hours. After natural cooling, the mixture was diluted with water and then extracted with toluene. After the toluene layer was concentrated, the residual component was purified with a silica gel column. As a result, 5.3 g of 3-iodo-9-ethylcarbazole was obtained (corresponding to a 65% yield).

後処理

  1. extractionextracted with toluene
  2. concentrationAfter the toluene layer was concentrated
  3. customthe residual component was purified with a silica gel column

出典と根拠

ORDレコード
ord-b37ac43a3c0243d18eb0c5bbdba4dfce
出典データセット
uspto-grants-1998_05
特許番号
US05756248

反応ノート

読み込み中…