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

HRID 975610

반응식

HRID 975610 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 68951,2,3-Trichlorobenzene

시약·촉매·용매 1

HCID 416358Bis(cyclopentadienyl)titanium(IV) chloride촉매

반응 조건

온도
96 °C

실험 절차

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 Aliquots were withdrawn by syringe, quenched with water, and extracted with diethyl ether.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.

후처리

  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 customAliquots were withdrawn by syringe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

출처 및 근거

ORD 기록
ord-afb72519c4d7429caf96dfaa4c7ee144
출처 데이터셋
uspto-grants-1997_03
특허 번호
US05608135

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