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Carbon Dioxide → 3-Dodecyl-alpha-phenyl-5-isoxazole acetic acid

HRID 264112
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HRID 264112 반응식
[CH2:1]([C:13]1[CH:17]=[C:16]([CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[O:15][N:14]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].C(C1ON=C(CC2C=CC=CC=2)C=1)CCCCCCCCCCC.C([Li])CCC.[C:54](=[O:56])=[O:55].C(C1ON=C(C(C2C=CC=CC=2)C(O)=O)C=1)CCCCCCCCCCC>O1CCCC1>[CH2:1]([C:13]1[CH:17]=[C:16]([CH:18]([C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=2)[C:54]([OH:56])=[O:55])[O:15][N:14]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]
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참가 물질

7

반응물 5

HCID 280Carbon Dioxide2회HCID 105232775-Dodecyl-alpha-phenyl-3-isoxazole acetic acidHCID 105682385-Dodecyl-3-(phenylmethyl)isoxazoleHCID 105923395-Benzyl-3-dodecylisoxazoleHCID 178418339Butyllithium

생성물 1

HCID 108330563-Dodecyl-alpha-phenyl-5-isoxazole acetic acid

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
-78 °C

실험 절차

To a cold (-78° C.), stirred suspension of 3-dodecyl-5-(phenylmethyl)isoxazole and 5-dodecyl-3-(phenylmethyl)isoxazole (1.64 g, 0.00500 mol) in dry tetrahydrofuran (150 mL) was added dropwise over 3 minutes a 2.06M solution (5.0 mL, 0.010 mol) of n-butyl lithium in hexanes, and the mixture was stirred for 80 minutes under nitrogen. The resulting orange solution was poured into freshly crushed dry ice (~300 g), the mixture was covered with parafilm with a small hole to allow CO2 (g) to escape, and allowed to warm to room temperature over 3 hours. The residue was partitioned between ether and 0.1M HCl. The organic layer was washed (saturated NaCl), dried (MgSO4), and rotoevaporated to a yellow oil. The oil was dissolved in petroleum ether (50 mL). A solid crystallized. It was filtered off and dried in vacuo to give a white solid containing the title compound and 5-dodecyl-α-phenyl-3-isoxazole acetic acid; yield 1.70 g (91%); mp 88°-97° C.

후처리

  1. stirringthe mixture was stirred for 80 minutes under nitrogen
  2. temperatureto warm to room temperature over 3 hours
  3. customThe residue was partitioned between ether and 0.1M HCl
  4. washThe organic layer was washed (saturated NaCl)
  5. dry with materialdried (MgSO4)
  6. dissolutionThe oil was dissolved in petroleum ether (50 mL)
  7. customA solid crystallized
  8. filtrationIt was filtered off
  9. customdried in vacuo
  10. customto give a white solid

출처 및 근거

ORD 기록
ord-96481a6d47f54c0988e9667632b27567
출처 데이터셋
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05646170

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