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Triethylamine → (S)-N-Methyl-2,3-dihydro-1H-inden-1-amine

HRID 552761
ノート
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反応式

HRID 552761 の反応式
[NH2:1][C@@H:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3]1.[CH3:11]CN(CC)CC.C(OC(OC(OC(C)(C)C)=O)=O)(C)(C)C>C1COCC1>[CH3:11][NH:1][C@@H:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 90495Di-tert-butyl dicarbonateHCID 70000841-Aminoindane, (S)-

生成物 1

HCID 15859055(S)-N-Methyl-2,3-dihydro-1H-inden-1-amine収率 77%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of (S)-(+)-1-aminoindan (176 mg, 1.29 mmol) in THF (10.0 mL) was added Et3N (0.200 mL, 1.43 mmol) followed by di-tert-butyldicarbonate (286 mg, 1.31 mmol). The mixture was stirred under an atmosphere of nitrogen for 3 days, concentrated, diluted with DCM (100 mL), and washed with 0.1 N aq hydrochloric acid (50.0 mL) and aq NaCl. The organic layer was dried (MgSO4), filtered and concentrated. The tan solid was taken up in tetrahydrofuran (10.0 mL) and to this was added with a 1.00 M solution of lithium aluminum hydride (1.0 M in THF, 5.80 mL). The mixture was heated at reflux for 6 hours, quenched with water (0.300 mL), 15% aq NaOH solution (0.300 mL) and water (0.900 mL). This was stirred for 10 minutes, filtered through celite, diluted with EtOAc (100 mL), dried (MgSO4), filtered and concentrated. The residue was purified via flash chromatography (0 to 100% EtOAc/hexanes to 10% MeOH/DCM) to afford the title compound as a black solid (146 mg, 77%).

後処理

  1. concentrationconcentrated
  2. additiondiluted with DCM (100 mL)
  3. washwashed with 0.1 N aq hydrochloric acid (50.0 mL) and aq NaCl
  4. dry with materialThe organic layer was dried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. additionto this was added with a 1.00 M solution of lithium aluminum hydride (1.0 M in THF, 5.80 mL)
  8. temperatureThe mixture was heated
  9. temperatureat reflux for 6 hours
  10. customquenched with water (0.300 mL), 15% aq NaOH solution (0.300 mL) and water (0.900 mL)
  11. stirringThis was stirred for 10 minutes
  12. filtrationfiltered through celite
  13. additiondiluted with EtOAc (100 mL)
  14. dry with materialdried (MgSO4)
  15. filtrationfiltered
  16. concentrationconcentrated
  17. customThe residue was purified via flash chromatography (0 to 100% EtOAc/hexanes to 10% MeOH/DCM)

出典と根拠

ORDレコード
ord-8ea25896b2a744c4af4acf12a6d65beb
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07951810B2

反応ノート

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