tert-Butyl mercaptan → 1,2,4,5-Tetrakis(tert-butylthio)benzene

HRID 1048731

反応式

HRID 1048731 の反応式
[Na].[CH3:2][C:3]([SH:6])([CH3:5])[CH3:4].Cl[C:8]1[CH:13]=[C:12](Cl)[C:11](Cl)=[CH:10][C:9]=1Cl>CN(C=O)C>[C:3]([S:6][C:8]1[CH:13]=[C:12]([S:6][C:3]([CH3:5])([CH3:4])[CH3:2])[C:11]([S:6][C:3]([CH3:5])([CH3:4])[CH3:2])=[CH:10][C:9]=1[S:6][C:3]([CH3:5])([CH3:4])[CH3:2])([CH3:5])([CH3:4])[CH3:2]

参加物

5

反応物 3

HCID 6387tert-Butyl mercaptanHCID 72701,2,4,5-TetrachlorobenzeneHCID 5360545Sodium

生成物 1

HCID 118120541,2,4,5-Tetrakis(tert-butylthio)benzene収率 69%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

Sodium (9.3 g, 0.18 mol) was added to a degassed solution of 2-methyl-2-propanethiol (20.9 mL, 0.18 mol) in dry DMF (105 mL), under stirring at 0° C. in nitrogen atmosphere. The mixture was allowed to reach room temperature (RT, 20-25° C.) and stirred overnight. 1,2,4,5-Tetrachlorobenzene (8.0 g, 0.037 mol) was then added and the resulting mixture was stirred at RT for 2 h and then gently refluxed for 18 h. After cooling at RT, the reaction mixture was poured over ice (100 g), the precipitate was removed by filtration, washed with water, and dried to give 11.0 g of the title compound as an off-white powder.

後処理

  1. customto reach room temperature
  2. custom(RT, 20-25° C.)
  3. stirringstirred overnight
  4. stirringthe resulting mixture was stirred at RT for 2 h
  5. temperaturegently refluxed for 18 h
  6. temperatureAfter cooling at RT
  7. customthe precipitate was removed by filtration
  8. washwashed with water
  9. customdried

出典と根拠

ORDレコード
ord-87b806a754504fe39d1e651f26080e47
出典データセット
uspto-grants-2016_07
特許番号
US09381257B2

関連ノート

読み込み中…