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Pyrrolidine → 7-pyrrolidin-1-yl-3,4-dihydro-2H-naphthalen-1-one

HRID 2089474
ノート
印刷プレビュー

反応式

HRID 2089474 の反応式
Br[C:2]1[CH:11]=[C:10]2[C:5]([CH2:6][CH2:7][CH2:8][C:9]2=[O:12])=[CH:4][CH:3]=1.[NH:13]1[CH2:17][CH2:16][CH2:15][CH2:14]1.C(P(C(C)(C)C)C1C=CC=CC=1C1C=CC=CC=1)(C)(C)C.CC(C)([O-])C.[Na+]>ClCCl.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.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C1(C)C=CC=CC=1>[N:13]1([C:2]2[CH:11]=[C:10]3[C:5]([CH2:6][CH2:7][CH2:8][C:9]3=[O:12])=[CH:4][CH:3]=2)[CH2:17][CH2:16][CH2:15][CH2:14]1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 31268PyrrolidineHCID 2527317-Bromo-1,2,3,4-tetrahydronaphthalen-1-oneHCID 27342152-(Di-tert-butylphosphino)biphenylHCID 23676156Sodium t-butoxide

生成物 1

HCID 591994477-pyrrolidin-1-yl-3,4-dihydro-2H-naphthalen-1-one

試薬・触媒・溶媒 3

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 1140Toluene溶媒
HCID 6344Dichloromethane溶媒

実験手順

A dry flask is charged with 7-bromo-3,4-dihydro-2H-naphthalen-1-one (CAS#32281-97-3, 0.102 g, 0.454 mmol), pyrrolidine (0.065 g, 0.909 mmol), 2-(di-t-butylphosphino)-biphenyl (0.020 g, 0.067 mmol), sodium tert-butoxide (0.087 g, 0.905 mmol) and toluene (3 mL). The flask is evacuated and filled with nitrogen three times. Pd2(dba)3 (0.041 g, 0.045 mmol) is added and the mixture is heated to reflux for 3 hours, whereupon the mixture is cooled to room temperature, diluted with dichloromethane and washed with water. The organic phase is dried over sodium sulfate and concentrated. The resulting residue is purified by silica gel chromatography (elution with hexanes-ethyl acetate mixtures) to give 7-pyrrolidin-1-yl-3,4-dihydro-2H-naphthalen-1-one; 1H NMR (400 MHz, CDCl3) δ ppm 1.99-2.03 (m, 4 H), 2.06-2.14 (m, 2 H), 2.60-2.65 (m, 2 H), 2.87 (t, J=6.1 Hz, 2 H), 3.28-3.35 (m, 4 H), 6.75 (dd, J=8.3, 2.8 Hz, 1 H), 7.12 (d, J=8.3 Hz, 1 H), 7.19 (d, J=2.8 Hz, 1 H).

後処理

  1. customThe flask is evacuated
  2. additionfilled with nitrogen three times
  3. temperaturethe mixture is heated
  4. temperatureto reflux for 3 hours, whereupon the mixture
  5. washwashed with water
  6. dry with materialThe organic phase is dried over sodium sulfate
  7. concentrationconcentrated
  8. customThe resulting residue is purified by silica gel chromatography (elution with hexanes-ethyl acetate mixtures)

出典と根拠

ORDレコード
ord-d7d36c28a99e4eb18bddf3838671b429
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08436035B2

反応ノート

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