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4,4'-Dichlorodiphenylmethane → 1,1'-(4-Chlorobutane-1,1-diyl)bis(4-chlorobenzene)

HRID 1700940
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HRID 1700940 반응식
[CH:1]1[C:6]([CH2:7][C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=2)=[CH:5][CH:4]=[C:3]([Cl:15])[CH:2]=1.C([Li])CCC.[Cl:21][CH2:22][CH2:23][CH2:24]I>O1CCCC1>[Cl:21][CH2:22][CH2:23][CH2:24][CH:7]([C:8]1[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=1)[C:6]1[CH:1]=[CH:2][C:3]([Cl:15])=[CH:4][CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 75764,4'-DichlorodiphenylmethaneHCID 813631-Chloro-3-iodopropaneHCID 178418339Butyllithium

생성물 1

HCID 183190411,1'-(4-Chlorobutane-1,1-diyl)bis(4-chlorobenzene)수율 44%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 4,4′-dichlorodiphenylmethane (4.37 g, 18.4 mmol) (Blackwell, J. et all, J. Chem. Soc., 1961, 1405) in dry tetrahydrofuran (50 ml) was treated at 0° C. with butyllithium (12.1 ml of 1.6 M, 19.36 mmol) added dropwise over 15 min. After 15 min, the red solution was then added dropwise to a cold (−78° C.) solution of 1-chloro-3-iodopropane (15.0 g, 73.4 mmol) in dry tetrahydrofuran (120 ml). After 20 min at −78° C., the reaction mixture was quenched by the addition of saturated ammonium chloride (100 ml) and diluted with toluene. The organic phase was washed with brine and dried. The oil obtained after evaporation of the solvent was purified on silica gel (elution hexane-toluene 85:15) and distilled under vacuum to give 2.54 g (44%) of the title material as a clear oil: bp 110-130° C./1.5 torr (air bath temperature).

후처리

  1. additionadded dropwise over 15 min
  2. waitAfter 20 min at −78° C.
  3. customthe reaction mixture was quenched by the addition of saturated ammonium chloride (100 ml)
  4. additiondiluted with toluene
  5. washThe organic phase was washed with brine
  6. customdried
  7. customThe oil obtained
  8. customafter evaporation of the solvent
  9. customwas purified on silica gel (elution hexane-toluene 85:15)
  10. distillationdistilled under vacuum

출처 및 근거

ORD 기록
ord-4906f058dea0494c8e6b83d9991829bf
출처 데이터셋
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06350892B1

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