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Diisopropylethylamine → 7-(3-ethyl-1,2,4-oxadiazol-5-yl)-1-(phenylsulfonyl)-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazine

HRID 2421897
ノート
印刷プレビュー

反応式

HRID 2421897 の反応式
[C:1]1([S:7]([N:10]2[CH2:15][CH2:14][O:13][C:12]3[N:16]=[CH:17][C:18]([C:20](Cl)=[O:21])=[CH:19][C:11]2=3)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O[NH:24][C:25](=[NH:28])[CH2:26][CH3:27].CCN(C(C)C)C(C)C>C(Cl)Cl.C1COCC1.CCCC[N+](CCCC)(CCCC)CCCC.[F-]>[CH2:26]([C:25]1[N:28]=[C:20]([C:18]2[CH:17]=[N:16][C:12]3[O:13][CH2:14][CH2:15][N:10]([S:7]([C:1]4[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=4)(=[O:9])=[O:8])[C:11]=3[CH:19]=2)[O:21][N:24]=1)[CH3:27]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 81531DiisopropylethylamineHCID 578966591-(phenylsulfonyl)-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazine-7-carbonyl chlorideHCID 178458070HCID 178458070、化合物

生成物 1

HCID 442428007-(3-ethyl-1,2,4-oxadiazol-5-yl)-1-(phenylsulfonyl)-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazine収率 64.4%

試薬・触媒・溶媒 3

HCID 6344Dichloromethane
溶媒
HCID 8028Tetrahydrofuran溶媒2 回
HCID 2724141Tetrabutylammonium Fluoride溶媒

実験手順

To a solution of 1-(phenylsulfonyl)-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazine-7-carbonyl chloride (40 mg, 0.118 mmol; Example 1, Step 1) in DCM (2 mL) was added N-hydroxypropionimidamide (20.81 mg, 0.236 mmol) and DIPEA (50 μL, 0.286 mmol). The reaction was stirred at room temperature for 16 hours. LCMS analysis of the reaction mixture indicated consumption of starting material. The reaction mixture was treated with saturated aqueous NaHCO3 (10 mL) and extracted with EtOAc (3×10 mL). The combined organics were dried over anhydrous Na2SO4 and concentrated in vacuo. The resulting solid was diluted with THF (5 mL) and TBAF in THF (118 μL, 0.118 mmol) was added. The reaction was then stirred overnight. The reaction mixture was concentrated in vacuo and the resulting paste was purified by flash column chromatography using a gradient elution of hexanes with 30-100% EtOAc to provide 7-(3-ethyl-1,2,4-oxadiazol-5-yl)-1-(phenylsulfonyl)-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazine (29.7 mg, 0.076 mmol, 64.2% yield) as a white solid. LCMS (+ESI) m/z=373.0 [M+H]+; 1H-NMR (CDCl3) δ 8.87 (d, 1H), 8.77 (d, 1H), 7.71 (m, 2H), 7.63 (tt, 1H) 7.51 (m, 2H), 4.01 (m, 2H), 3.92 (m, 2H), 2.84 (q, 2H), 1.39 (t, 3H).

後処理

  1. customconsumption of starting material
  2. additionThe reaction mixture was treated with saturated aqueous NaHCO3 (10 mL)
  3. extractionextracted with EtOAc (3×10 mL)
  4. dry with materialThe combined organics were dried over anhydrous Na2SO4
  5. concentrationconcentrated in vacuo
  6. additionwas added
  7. stirringThe reaction was then stirred overnight
  8. concentrationThe reaction mixture was concentrated in vacuo
  9. customthe resulting paste was purified by flash column chromatography
  10. washa gradient elution of hexanes with 30-100% EtOAc

出典と根拠

ORDレコード
ord-0e6e740a9e5543da87ce3b21c85fde6a
出典データセット
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07960377B2

反応ノート

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