反応 #7044

ord-4dd0bc4fe8c64d9e8f8801e446e2f232

反応方程式

CCCC(c1c[nH]c2ccccc12)c1c[nH]c2ccccc12
1,1-di-indol-3-yl-butane
ClCc1ccccc1
benzylchloride
CCCC(c1cn(Cc2ccccc2)c2ccccc12)c1cn(Cc2ccccc2)c2ccccc12
product
収率 78.0%
CCCC(c1cn(Cc2ccccc2)c2ccccc12)c1cn(Cc2ccccc2)c2ccccc12
1,1-di-(N-benzyl-indol-3-yl)-butane
収率 78.0%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The mixture thus obtained
  2. 2
    workup.STIRRINGthe ultrasonic stirring
  3. 3
    その他the chloroform phase was separated
  4. 4
    洗浄washed with a small amount of water
  5. 5
    その他dried on Na2SO4
  6. 6
    ろ過filtered
  7. 7
    濃縮concentrated to dryness
  8. 8
    その他The end product was isolated
  9. 9
    その他purified chromatographically on silica gel
  10. 10
    洗浄eluting with hexane

実験手順

ST 1385 1,1-di-indol-3-yl-butane, 290 mg (1 mmol), was thoroughly mixed and blended with potassium tertbutylate (280 mg) and tetrabutylammonium bromide (20 mg). The mixture thus obtained was held under ultrasonic stirring at ambient temperature. 640 mg (5 mmol) of benzylchloride at 0° C. were then added and the ultrasonic stirring was continued for 2 hours at room temperature. At the end of this period, the reaction mixture was treated with H2O/CHCl3; the chloroform phase was separated, washed with a small amount of water, dried on Na2SO4, filtered and concentrated to dryness. The end product was isolated and purified chromatographically on silica gel, eluting with hexane:ethyl ether 95:5.351 mg of product were obtained with a 78% yield.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07084166B2uspto-grants-2006_08