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(R)-5-(2-Ethylsulphonylethenyl)-3-(N-methylpyrrolidin-2-ylmethyl)-1H-indole → (R)-5-(2-Ethylsulphonylethyl)-3-(N-methylpyrrolidin-2-ylmethyl)1H-indole

HRID 745010
ノート
印刷プレビュー

反応式

HRID 745010 の反応式
[CH2:1]([S:3]([CH:6]=[CH:7][C:8]1[CH:9]=[C:10]2[C:14](=[CH:15][CH:16]=1)[NH:13][CH:12]=[C:11]2[CH2:17][C@H:18]1[CH2:22][CH2:21][CH2:20][N:19]1[CH3:23])(=[O:5])=[O:4])[CH3:2]>Cl.CN(C)C=O.O.[Pd]>[CH2:1]([S:3]([CH2:6][CH2:7][C:8]1[CH:9]=[C:10]2[C:14](=[CH:15][CH:16]=1)[NH:13][CH:12]=[C:11]2[CH2:17][C@H:18]1[CH2:22][CH2:21][CH2:20][N:19]1[CH3:23])(=[O:5])=[O:4])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 1

HCID 54504320(R)-5-(2-Ethylsulphonylethenyl)-3-(N-methylpyrrolidin-2-ylmethyl)-1H-indole

生成物 1

HCID 9884122(R)-5-(2-Ethylsulphonylethyl)-3-(N-methylpyrrolidin-2-ylmethyl)1H-indole収率 69.6%

試薬・触媒・溶媒 4

HCID 23938Palladium触媒HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒
HCID 6228
Dimethylformamide
溶媒

実験手順

(R)-5-(2-Ethylsulphonylethenyl)-3-(N-methylpyrrolidin-2-ylmethyl)-1H-indole (157 mg) was dissolved in a mixture of ethanolic hydrogen chloride [prepared by addition of acetyl chloride (0.043 mL) to ethanol (10 mL)], N,N-dimethylformamide (7.5 mL) and water (0.1 mL) and the solution was shaken under a hydrogen atmosphere (15 psi) at room temperature for 18 hours in the presence of 10% palladium on carbon (150 mg). The mixture was filtered through Arbacel (trade mark) filter aid and the residue was washed well with ethanol. The combined filtrate and washings were evaporated under reduced pressure and the residual oil was partitioned between ethyl acetate and 2M aqueous sodium carbonate solution. The organic layer was separated, washed three times with water followed by brine and then dried (Na2SO4). Evaporation of the solvent gave an oil which was chromatographed on silica gel. Elution with dichloromethane/methanol/concentrated aqueous ammonia (90:10:1) gave the title compound as a gum (110 mg): TLC (CH2Cl2 /C2H5OH/NH3 ; 90:10:1): Rf =0.3; [α]25D =+62° (methanol, c=0.10). Anal. Calcd for C18H26N2O2S. 0.05 CH2Cl2:C,63.21; H,7.67; N,8.17. Found: C,63.55; H,7.61; N,8.41.

後処理

  1. filtrationThe mixture was filtered through Arbacel (trade mark)
  2. filtrationfilter aid
  3. washthe residue was washed well with ethanol
  4. customThe combined filtrate and washings were evaporated under reduced pressure
  5. customthe residual oil was partitioned between ethyl acetate and 2M aqueous sodium carbonate solution
  6. customThe organic layer was separated
  7. washwashed three times with water
  8. dry with materialdried (Na2SO4)
  9. customEvaporation of the solvent
  10. customgave an oil which
  11. customwas chromatographed on silica gel
  12. washElution with dichloromethane/methanol/concentrated aqueous ammonia (90:10:1)

出典と根拠

ORDレコード
ord-74913499aaf343f1bb4e1b9b19b7ecbf
出典データセット
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05559246

反応ノート

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