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Methanol → (S)-2-(3-phenoxy-phenyl)-pyrrolidine

HRID 29069
ノート
印刷プレビュー

反応式

HRID 29069 の反応式
C1([SiH3])C=CC=CC=1.N1CCCC1.CO.[O:15]([C:22]1[CH:23]=[C:24]([C:28]2[CH2:29][CH2:30][CH2:31][N:32]=2)[CH:25]=[CH:26][CH:27]=1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>C1COCC1>[O:15]([C:22]1[CH:23]=[C:24]([C@@H:28]2[CH2:29][CH2:30][CH2:31][NH:32]2)[CH:25]=[CH:26][CH:27]=1)[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=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 887MethanolHCID 12752PhenylsilaneHCID 31268PyrrolidineHCID 597880425-(3-phenoxy-phenyl)-3,4-dihydro-2H-pyrrole

生成物 1

HCID 59787976(S)-2-(3-phenoxy-phenyl)-pyrrolidine収率 48%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To oven dried round bottom flask is added S,S-EBTHITiF2 (100 mgs, 0.3 mmol) and diluted with THF (5 mL). The flask is sealed and purged with argon. To the yellow solution is added phenylsilane (4.6 mL, 37.5 mmol), pyrrolidine (100 uL, 1.1 mmol), and anhydrous methanol (100 uL, 1.1 mmol). The resulting yellow mixture is stirred for 45 minutes until green color persisted. A solution of 5-(3-phenoxy-phenyl)-3,4-dihydro-2H-pyrrole (1.2 g, 5.05 mmol) in THF (2 mL) is added to the catalyst and the mixture is stirred for 8 hrs. The reaction is carefully quenched with 10% HCl (100 mL) until gas evolution subsided and the pH˜2. The mixture is diluted with EtOAc (100 mL) and the aqueous layer is removed, neutralized with 3M NaOH (50 mL) until basic and extracted with EtOAc (3×100 mL). The organics were combined, dried over Na2SO4, filtered and concentrated under reduced pressures. The solid residue is purifed by silica gel column chromatography (100% EtOAc) to give (S)-2-(3-phenoxy-phenyl)-pyrrolidine as a yellow solid (580 mgs, 48%). LCMS m/z 240.1 (M+1).

後処理

  1. customTo oven dried round bottom flask
  2. additionis added
  3. addition(100 mgs, 0.3 mmol) and diluted with THF (5 mL)
  4. customThe flask is sealed
  5. custompurged with argon
  6. stirringthe mixture is stirred for 8 hrs
  7. customThe reaction is carefully quenched with 10% HCl (100 mL) until gas evolution
  8. additionThe mixture is diluted with EtOAc (100 mL)
  9. customthe aqueous layer is removed
  10. extractionextracted with EtOAc (3×100 mL)
  11. dry with materialdried over Na2SO4
  12. filtrationfiltered
  13. concentrationconcentrated under reduced pressures

出典と根拠

ORDレコード
ord-a8c8fc737a0a4d49b25325644b24f3db
出典データセット
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07419975B2

反応ノート

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