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4-Fluorobenzylamine → HCID 68432621、化合物

HRID 1162844
ノート
印刷プレビュー

反応式

HRID 1162844 の反応式
[CH2:1]([O:8][CH2:9][CH:10]([NH:13][C:14](=[O:20])[O:15][C:16]([CH3:19])([CH3:18])[CH3:17])[CH:11]=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[F:21][C:22]1[CH:29]=[CH:28][C:25]([CH2:26][NH2:27])=[CH:24][CH:23]=1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C([O-])(O)=O.[Na+]>C1COCC1>[CH2:1]([O:8][CH2:9][CH:10]([NH:13][C:14](=[O:20])[O:15][C:16]([CH3:19])([CH3:18])[CH3:17])[CH2:11][NH:27][CH2:26][C:25]1[CH:28]=[CH:29][C:22]([F:21])=[CH:23][CH:24]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH: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

6

反応物 4

HCID 673264-FluorobenzylamineHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 14523252HCID 14523252、化合物

生成物 1

HCID 68432621HCID 68432621、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of tert-butyl 2-(benzyloxy)-1-formylethylcarbamate (3.29 g, 11.8 mmol) in anhydrous THF (12 mL) was added 4-fluorobenzylamine (2.03 mL, 17.7 mmol). After 10 min, sodium triacetoxyborohydride (3.99 g, 18.8 mmol) was added, and the reaction was stirred at ambient temperature under inert atmosphere for 30 min. Saturated aqueous NaHCO3 solution was added and the mixture stirred until gas evolution ceased. The aqueous layer was extracted with EtOAc, saturated with NaCl and again extracted with EtOAc. The combined organic extracts were washed with brine, dried over Na2SO4 and concentrated in vacuo. The resulting cloudy yellow oil was purified by silica gel chromatography (EtOAc to 10% MeOH/EtOAc) to afford the title compound as a pale yellow oil. 1H NMR (500 MHz, CDCl3) δ 7.37-7.23 (m, 7H), 7.03-6.96 (m, 2H), 5.04 (br s, 1H), 4.49 (dd, J=11.5, 18.0 Hz, 2H), 3.86 (br s, 1H), 3.76-3.70 (m, 2H), 3.60 (dd, J=3.0, 9.0 Hz, 1H), 3.53 (d, J=4.5 Hz, 1H), 2.83-2.80 (m, 1H), 2.76-2.72 (m, 1H), 1.44 (s, 9H). ES MS (M+1)=389.5.

後処理

  1. stirringthe mixture stirred until gas evolution
  2. extractionThe aqueous layer was extracted with EtOAc, saturated with NaCl
  3. extractionagain extracted with EtOAc
  4. washThe combined organic extracts were washed with brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated in vacuo
  7. customThe resulting cloudy yellow oil was purified by silica gel chromatography (EtOAc to 10% MeOH/EtOAc)

出典と根拠

ORDレコード
ord-10b575656c084260a621688aefe929fe
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07820680B2

反応ノート

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