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Triphenylphosphine → 1'-pentylspiro[furo[2,3-f][1,3]benzodioxole-7,3'-pyrrolo[2,3-b]pyridin]-2'(1'H)-one

HRID 1715222
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HRID 1715222 반응식
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O.O[C:33]1[C:34]([C:42]2([CH2:57][OH:58])[C:50]3[C:45](=[N:46][CH:47]=[CH:48][CH:49]=3)[N:44]([CH2:51][CH2:52][CH2:53][CH2:54][CH3:55])[C:43]2=[O:56])=[CH:35][C:36]2[O:40][CH2:39][O:38][C:37]=2[CH:41]=1>C1COCC1>[CH2:51]([N:44]1[C:45]2=[N:46][CH:47]=[CH:48][CH:49]=[C:50]2[C:42]2([C:34]3=[CH:35][C:36]4[O:40][CH2:39][O:38][C:37]=4[CH:41]=[C:33]3[O:58][CH2:57]2)[C:43]1=[O:56])[CH2:52][CH2:53][CH2:54][CH3:55]
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참가 물질

5

반응물 3

HCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 119628123-(6-hydroxy-1,3-benzodioxol-5-yl)-3-(hydroxymethyl)-1-pentyl-1,3-dihydro-2H-pyrrolo[2,3-b]pyridin-2-one

생성물 1

HCID 118483031'-pentylspiro[furo[2,3-f][1,3]benzodioxole-7,3'-pyrrolo[2,3-b]pyridin]-2'(1'H)-one수율 54%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매
2회

실험 절차

To a mixture of triphenylphosphine (2.61 g, 9.95 mmol) and diethyl azodicarboxylate (1.73 g, 9.95 mmol) in anhydrous THF (100 mL) was added slowly a solution of 3-(6-hydroxy-1,3-benzodioxol-5-yl)-3-(hydroxymethyl)-1-pentyl-1,3-dihydro-2H-pyrrolo[2,3-b]pyridin-2-one (2.85 g, 7.69 mmol) in anhydrous THF (50.0 mL) at 0° C. The brown reaction solution was stirred at ambient temperature for 16 h and quenched with saturated ammonium chloride (50.0 mL). The organic solvent was removed under reduced pressure. The aqueous layer was extracted with ethyl acetate (100 mL). The organic solution was dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated in vacuo to dryness. The residue was subjected to column chromatography to give the title compound (1.45 g, 54%), which was triturated from ether and hexane to give a colorless solid: mp 126-127° C.; 1H NMR (300 MHz, CDCl3) δ 8.18 (dd, 1H), 7.54 (dd, 1H), 7.01 (dd, 1H), 6.666 (s, 1H), 6.25 (s, 1H), 5.89 (d, 1H), 4.71 (ABq, 2H), 3.68 (t, 2H), 1.70-1.60 (m, 2H), 1.32-1.22 (m, 4H), 0.82 (t, 3H); 13C NMR (75 MHz, CDCl3) δ 176.9, 156.8, 156.0, 149.0, 147.9, 142.3, 132.0, 126.7, 119.3, 119.2, 103.4, 101.9, 93.8, 79.7, 57.4, 39.3, 28.9, 27.1, 22.2, 14.3; MS (ES+, m/z) 353 (M+1).

후처리

  1. customquenched with saturated ammonium chloride (50.0 mL)
  2. customThe organic solvent was removed under reduced pressure
  3. extractionThe aqueous layer was extracted with ethyl acetate (100 mL)
  4. dry with materialThe organic solution was dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated in vacuo to dryness

출처 및 근거

ORD 기록
ord-bef4b5b9c8ae4a73bbd37709b534ac92
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07799798B2

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