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1-Bromo-3-fluorobenzene → ((S)-1-benzylpyrrolidin-3-yl)-(3-fluorophenyl)amine

HRID 660101
ノート
印刷プレビュー

反応式

HRID 660101 の反応式
[CH2:1]([N:8]1[CH2:12][CH2:11][C@H:10]([NH2:13])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Br[C:15]1[CH:16]=[C:17]([F:21])[CH:18]=[CH:19][CH:20]=1.CC(C)([O-])C.[Na+]>C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].C1(P(C2C=CC=CC=2)C2C=CC3C(=CC=CC=3)C=2C2C3C(=CC=CC=3)C=CC=2P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(C)C=CC=CC=1>[CH2:1]([N:8]1[CH2:12][CH2:11][C@H:10]([NH:13][C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([F:21])[CH:16]=2)[CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 140821-Bromo-3-fluorobenzeneHCID 1519353(3S)-(+)-1-Benzyl-3-aminopyrrolidineHCID 23676156Sodium t-butoxide

生成物 1

HCID 29080908((S)-1-benzylpyrrolidin-3-yl)-(3-fluorophenyl)amine収率 88.8%

試薬・触媒・溶媒 3

HCID 634876Binap, (A+-)-触媒
HCID 6505921
(1E,4E)-1,5-diphenylpenta-1,4-dien-3-one; palladium
触媒
HCID 1140Toluene溶媒

実験手順

A toluene solution containing 2.2 g of (S)-1-benzylpyrrolidin-3-ylamine (12.5 mmol), 2.2 g of 3-bromofluorobenzene (12.5 mmol), 0.31 g of 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (BINAP, 0.51 mmol), 0.14 g of bis(dibenzylideneacetone)palladium (Pd(dba)2, 0.22 mmol), and 1.3 g of sodium tert-butoxide (13.2 mmol) was heated under reflux under a nitrogen atmosphere for 3 hours. The reaction solution was filtered to remove insoluble matter, and ethyl acetate and water were added to the filtrate to separate the solution into layers. The organic layer was washed with water, the solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=20:1→1:1). The eluent solvent was distilled off under reduced pressure to thereby obtain 3.0 g of oily colorless ((S)-1-benzylpyrrolidin-3-yl)-(3-fluorophenyl)amine.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux under a nitrogen atmosphere for 3 hours
  3. filtrationThe reaction solution was filtered
  4. customto remove insoluble matter, and ethyl acetate and water
  5. additionwere added to the filtrate
  6. customto separate the solution into layers
  7. washThe organic layer was washed with water
  8. distillationthe solvent was distilled off under reduced pressure
  9. customthe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=20:1→1:1)
  10. distillationThe eluent solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-eb5add572dfd45ce871c0484e23348c1
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08084442B2

反応ノート

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