Tert-Butylbenzene → HCID 22625489、化合物

HRID 277689

反応式

HRID 277689 の反応式
[I:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1)=O.[F:9][C:10]([F:21])([F:20])[CH:11]([F:19])[C:12]([F:18])([F:17])[S:13]([OH:16])(=[O:15])=[O:14].[C:22]([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)([CH3:25])([CH3:24])[CH3:23]>ClCCl>[F:21][C:10]([F:9])([F:20])[CH:11]([F:19])[C:12]([F:17])([F:18])[S:13]([O-:16])(=[O:14])=[O:15].[C:22]([C:26]1[CH:31]=[CH:30][C:29]([I+:1][C:3]2[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=2)=[CH:28][CH:27]=1)([CH3:25])([CH3:24])[CH3:23]

参加物

5

反応物 3

HCID 7366Tert-ButylbenzeneHCID 92125IodosylbenzeneHCID 97946281-Propanesulfonic acid, 1,1,2,3,3,3-hexafluoro-

生成物 1

HCID 22625489HCID 22625489、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

4.4 g (20 mmol) of iodosylbenzene was suspended in 100 ml of dry dichloromethane. The suspension was cooled to 0° C. with stirring. 4.65 g (20 mmol) of 3,3,3,2,1,1-hexafluoropropane sulfonic acid (optionally distilled) was added at the same temperature thereto under exclusion of moisture. The mixture was stirred at room temperature for 3 hours. The temperature of the mixture was returned to 0° C., and 2.68 g (20 mmol) of 4-t-butylbenzene was added thereto at that temperature. The temperature of the mixture was returned to room temperature, followed by stirring for 6 hours. Thereafter, the insolubles were removed by filtration. The solvent was removed from the filtrate. The oily residue was purified by recrystallization (twice) from diethyl ether. The structure was confirmed by 1H-NMR (CDCl3): δ=0.81 (s, 9H), 4.98-5.22 (m[d], 1H), 7.18-7.23 (d, 2H), 7.58-7.65 ppm (m, 7H).

後処理

  1. additionwas added at the same temperature
  2. stirringThe mixture was stirred at room temperature for 3 hours
  3. customwas returned to 0° C.
  4. customwas returned to room temperature
  5. stirringby stirring for 6 hours
  6. customThereafter, the insolubles were removed by filtration
  7. customThe solvent was removed from the filtrate
  8. customThe oily residue was purified by recrystallization (twice) from diethyl ether

出典と根拠

ORDレコード
ord-10b1fad91dc64ce68db68fd3e18524a1
出典データセット
uspto-grants-2002_03
特許番号
US06358665B1

関連ノート

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