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3-Phenylphenol → N-tert-Butoxycarbonyl-trans-4-(3-Biphenyloxy)-L-Proline Methyl Ester

HRID 2185493
ノート
印刷プレビュー

反応式

HRID 2185493 の反応式
[CH3:1]COC(/N=N/C(OCC)=O)=O.[C:13]([O:17][C:18]([N:20]1[CH2:27][C@H:26]([OH:28])[CH2:25][C@H:21]1[C:22]([OH:24])=[O:23])=[O:19])([CH3:16])([CH3:15])[CH3:14].[C:29]1([C:35]2[CH:36]=[C:37](O)[CH:38]=[CH:39][CH:40]=2)[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>O1CCCC1>[CH3:1][O:23][C:22](=[O:24])[C@@H:21]1[CH2:25][C@@H:26]([O:28][C:31]2[CH:30]=[C:29]([C:35]3[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=3)[CH:34]=[CH:33][CH:32]=2)[CH2:27][N:20]1[C:18]([O:17][C:13]([CH3:16])([CH3:14])[CH3:15])=[O:19]
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 113813-PhenylphenolHCID 11776TriphenylphosphineHCID 88804(2S,4R)-4-hydroxy-1-[(2-methylpropan-2-yl)oxycarbonyl]pyrrolidine-2-carboxylic acidHCID 5462977Diethyl azodicarboxylate

生成物 1

HCID 21341533N-tert-Butoxycarbonyl-trans-4-(3-Biphenyloxy)-L-Proline Methyl Ester

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒
2 回

実験手順

A solution of diethylazodicarboxylate (829 μL) in tetrahydrofuran (10 mL) was added to a cold (−15° C.) stirred solution of N-tert-butoxycarbonyl-trans-4-hydroxy-L-proline (1.23 g), 3-phenylphenol (896 mg), and triphenyl phosphine (1.38 g) in tetrahydrofuran (30 mL) under argon, After stirring at room temperature for 15.5 hr, the solvent was evaporated and coevaporated several times with toluene in vacuo. The residue was diluted with toluene and precipitated solids were removed by filtration, which was washed with toluene. The combined organic layers were evaporated in vacuo and the residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:10, v/v) to give title compound (837 mg): 1H-NMR (400 MHz, CDCl3) δ 1.36-1.50 (m, 9H), 2.18-2.29 (m, 1H), 2.51-2.64 (m, 1H), 3.68-3.89 (m, 5H), 4.40-4.56 (m, 1H), 4.91-5.01 (m, 1H), 6.79-6.87 (m, 1H), 7.04-7.10 (m, 1H), 7.17-7.24 (m, 1H), 7.29-7.39 (m, 2H), 7.39-7.49 (m, 2H), and 7.49-7.60 (m, 2H).

後処理

  1. customthe solvent was evaporated
  2. additionThe residue was diluted with toluene
  3. customprecipitated solids
  4. customwere removed by filtration, which
  5. washwas washed with toluene
  6. customThe combined organic layers were evaporated in vacuo
  7. customthe residue was purified by silica gel column chromatography (ethyl acetate

出典と根拠

ORDレコード
ord-f9e90175c4d644828eb67129e09eb16b
出典データセット
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06399629B1

反応ノート

読み込み中…

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