1,2,4,5-Tetrachlorobenzene → 1,2,3-Trichlorobenzene

HRID 975610

反応式

HRID 975610 の反応式
Cl[C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([Cl:9])=[CH:4][C:3]=1Cl.[BH4-].[Na+].[Cl-:13].[Li+]>[CH-]1[C-]=[C-][C-]=[C-]1.[CH-]1[C-]=[C-][C-]=[C-]1.Cl[Ti]Cl>[Cl:8][C:6]1[C:5]([Cl:9])=[C:4]([Cl:13])[CH:3]=[CH:2][CH:7]=1

参加物

5

反応物 3

HCID 72701,2,4,5-TetrachlorobenzeneHCID 433294Lithium ChlorideHCID 4311764Sodium borohydride

生成物 1

HCID 68951,2,3-Trichlorobenzene

試薬・触媒・溶媒 1

HCID 416358Bis(cyclopentadienyl)titanium(IV) chloride触媒

反応条件

温度
96 °C

実験手順

A flask equipped with a magnetic stir bar and a water cooled condenser with an oil bubbler was charged with 1,2,4,5-tetrachlorobenzene (648 mg, 3.0 mmol), sodium tetrahydridoborate (1135 mg, 30.0 mmol), bis(η5 -cyclopentadienyl)titanium dichloride (75 mg, 0.3 mmol) and 1-methyl-2pyrrolidine (NMP; 30.0 ml). The reaction mixture was heated at 96° C. in an oil bath. After 4.25 hours, lithium chloride (1.09 g, 30.0 mmol) was added. Aliquots were withdrawn by syringe, quenched with water, and extracted with diethyl ether. The ether layer was analyzed with the results shown in the following table. Only trichlorobenzene was produced.

後処理

  1. customA flask equipped with a magnetic stir bar and a water cooled condenser with an oil bubbler
  2. customAliquots were withdrawn by syringe
  3. customquenched with water
  4. extractionextracted with diethyl ether

出典と根拠

ORDレコード
ord-afb72519c4d7429caf96dfaa4c7ee144
出典データセット
uspto-grants-1997_03
特許番号
US05608135

関連ノート

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