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Lithium diisopropylamide → (S)-1-(2-Azido-benzoyl)-5-oxo-pyrrolidine-2-carboxylic acid tert-butyl ester

HRID 2427822
ノート
印刷プレビュー

反応式

HRID 2427822 の反応式
[C:1]([O:5][C:6](=[O:13])[C@@H:7]1[CH2:11][CH2:10][C:9](=[O:12])[NH:8]1)([CH3:4])([CH3:3])[CH3:2].[Li+].CC([N-]C(C)C)C.[N:22]([C:25]1[CH:33]=[CH:32][CH:31]=[CH:30][C:26]=1[C:27](Cl)=[O:28])=[N+:23]=[N-:24]>C1COCC1>[C:1]([O:5][C:6]([C@@H:7]1[CH2:11][CH2:10][C:9](=[O:12])[N:8]1[C:27](=[O:28])[C:26]1[CH:30]=[CH:31][CH:32]=[CH:33][C:25]=1[N:22]=[N+:23]=[N-:24])=[O:13])([CH3:4])([CH3:2])[CH3:3]
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 2724682Lithium diisopropylamideHCID 10888648tert-Butyl 5-oxo-L-prolinateHCID 117452552-Azidobenzoyl chloride

生成物 1

HCID 58096224(S)-1-(2-Azido-benzoyl)-5-oxo-pyrrolidine-2-carboxylic acid tert-butyl ester収率 82%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A stirred solution of (2S)-5-oxo-proline tert-butyl ester (T. Kolasa and M. J. Miller, J. Org. Chem., 1990, 55, 1711-1721) (1.13 g, 6.13 mmol) in anhydrous THF (15 mL) was treated at −78° C. with LDA (9.19 mmol) and the reaction was stirred for 15 min. A solution of 2-azidobenzoyl chloride (T. Okawa, T. Sugimori, S. Eguchi and A. Kakehi, Heterocycles, 1998, 47, 1, 375-382) (6.13 mmol) in anhydrous THF (5 mL) was then added dropwise and the reaction mixture was stirred at −78° C. for 1 h before being quenched with saturated aq.NH4Cl. The reaction was allowed to warm to room temperature and the organic layer was washed with saturated aq.NH4Cl, dried (MgSO4), filtered and evaporated to give an oil which was purified by flash chromatography (20% ethyl acetate in hexane) to afford the title compound as a pale yellow oil (1.67 g, 82%): 1H NMR (400 MHz, CDCl3) δ 1.53 (9H, s), 2.14 (1H, m), 2.43 (1H, m), 2.55 (1H, m), 2.69 (1H, m), 4.79 (1H, dd, J 9.2, 3.2 Hz), 7.19-7.22 (2H, m), 7.36 (1H, m), 7.49 (1H, m). 13C NMR (100 MHz, CDCl3) δ 22.1 (CH2), 28.3 (CH3), 31.9 (CH2), 59.3 (CH), 83.0 (C), 118.7 (CH), 125.0 (CH), 127.9 (C), 129.1 (CH), 131.9 (CH), 137.9 (C), 167.5 (C), 170.2 (C), 173.6 (C).

後処理

  1. stirringthe reaction mixture was stirred at −78° C. for 1 h
  2. custombefore being quenched with saturated aq
  3. washthe organic layer was washed with saturated aq
  4. dry with materialNH4Cl, dried (MgSO4)
  5. filtrationfiltered
  6. customevaporated
  7. customto give an oil which
  8. customwas purified by flash chromatography (20% ethyl acetate in hexane)

出典と根拠

ORDレコード
ord-41af7c072eec49108ba4aa9f962f922d
出典データセット
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07968716B2

反応ノート

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