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1-(4-Bromobenzyl)pyrrolidine → [3-Hydroxy-3-(4-pyrrolidin-1-ylmethyl-phenyl)-cyclobutyl]-morpholin-4-yl-methanone

HRID 1943261
ノート
印刷プレビュー

反応式

HRID 1943261 の反応式
Br[C:2]1[CH:13]=[CH:12][C:5]([CH2:6][N:7]2[CH2:11][CH2:10][CH2:9][CH2:8]2)=[CH:4][CH:3]=1.CC(C)=O.C(=O)=O.[Li]CCCC.[N:26]1([C:32]([CH:34]2[CH2:37][C:36](=[O:38])[CH2:35]2)=[O:33])[CH2:31][CH2:30][O:29][CH2:28][CH2:27]1>C1COCC1>[OH:38][C:36]1([C:2]2[CH:13]=[CH:12][C:5]([CH2:6][N:7]3[CH2:11][CH2:10][CH2:9][CH2:8]3)=[CH:4][CH:3]=2)[CH2:37][CH:34]([C:32]([N:26]2[CH2:31][CH2:30][O:29][CH2:28][CH2:27]2)=[O:33])[CH2:35]1
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 4

HCID 127380041-(4-Bromobenzyl)pyrrolidineHCID 18522661Acetone cardiceHCID 672785063-(Morpholin-4-ylcarbonyl)cyclobutanoneHCID 178418339Butyllithium

生成物 1

HCID 67279238[3-Hydroxy-3-(4-pyrrolidin-1-ylmethyl-phenyl)-cyclobutyl]-morpholin-4-yl-methanone収率 20.4%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

To a stirring solution of 1-(4-bromo-benzyl)-pyrrolidine (1.6 g, 6.5 mmol) in THF (20 mL) at −78° C. (acetone/dry ice bath) was added slowly down the side of the flask a solution of nBuLi (2.6 mL, 6.5 mmol, 2.5 M THF). After 15 minutes a solution of Intermediate 7, 3-(morpholin-4-ylcarbonyl)cyclobutanone (1.0 g, 5.4 mmol, in 7 mL of THF) precooled to −78° C. was added slowly. After 30 minutes the reaction was quenched cold with 1N HCl (20 mL). This mixture was diluted with EtOAc and then the layers were separated and the organic layer was discarded. The aqueous layer was basified with 1N NaOH and extracted with CHCl3/iPrOH (3:1). The organic layer was dried over MgSO4, filtered and concentrated to give a yellow oil. This material was purified by flash column chromatography using a 40 g ISCO™ column, eluting with a gradient of 3%, 5%, 10%, 20%, 30%/0 MeOH/CHCl3 with 0.1% NH4OH. The product containing fraction were collected and concentrated under reduced pressure to give the title compound (379 mg, 20% yield): Rf=0.3 (30% MeOH/CH2Cl2); LRMS m/z Calcd for C20H28N2O3, 344.4, found, 345 (M+1) APCI; 400 MHz 1H NMR (CDCl3) δ 7.42 (d, J=8.3 Hz, 2H), 7.29 (d, J=8.3 Hz, 2H), 4.58 (brs, 1H), 3.62-3.55 (m, 8H), 3.34-3.32 (m, 2H), 2.87 (dddd, J=8.3, 8.3, 8.3, 8.3 Hz, 1H), 2.77-2.71 (m, 2H), 2.64-2.59 (m, 2H), 2.48-2.45 (m, 4H), 1.75-1.70 (m, 4H); 100 MHz 13C NMR (CDCl3) δ 173.8, 144.4, 137.8, 129.3, 125.3, 72.9, 67.0, 66.9, 60.3, 54.2, 46.0, 42.6, 40.9, 28.1, 23.5.

後処理

  1. additionwas added slowly
  2. customAfter 30 minutes the reaction was quenched cold with 1N HCl (20 mL)
  3. additionThis mixture was diluted with EtOAc
  4. customthe layers were separated
  5. extractionextracted with CHCl3/iPrOH (3:1)
  6. dry with materialThe organic layer was dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customto give a yellow oil
  10. customThis material was purified by flash column chromatography
  11. washeluting with a gradient of 3%, 5%, 10%, 20%, 30%/0 MeOH/CHCl3 with 0.1% NH4OH
  12. additionThe product containing fraction
  13. customwere collected
  14. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-1320b05293204f259abe7fc3b31f1ded
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08389743B2

反応ノート

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