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Triethylamine → 2-(3-Dodecyl-isoxazol-5-yl)-2-phenyl-N-(2,4,6-trimethoxy-phenyl)-acetamide

HRID 1756969
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HRID 1756969 반응식
[CH2:1]([C:13]1[CH:17]=[C:16]([CH:18]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:19]([OH:21])=O)[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(C(C2C=CC=CC=2)C(O)=O)C=1)CCCCCCCCCCC.C(N1C=CN=C1)(N1C=CN=C1)=O.Cl.[CH3:68][O:69][C:70]1[CH:76]=[C:75]([O:77][CH3:78])[CH:74]=[C:73]([O:79][CH3:80])[C:71]=1[NH2:72].C(N(CC)CC)C>O1CCCC1>[CH2:1]([C:13]1[CH:17]=[C:16]([CH:18]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:19]([NH:72][C:71]2[C:73]([O:79][CH3:80])=[CH:74][C:75]([O:77][CH3:78])=[CH:76][C:70]=2[O:69][CH3:68])=[O:21])[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 8471TriethylamineHCID 682631,1'-CarbonyldiimidazoleHCID 27644342,4,6-trimethoxyaniline HydrochlorideHCID 105232775-Dodecyl-alpha-phenyl-3-isoxazole acetic acidHCID 108330563-Dodecyl-alpha-phenyl-5-isoxazole acetic acid

생성물 1

HCID 10075862
2-(3-Dodecyl-isoxazol-5-yl)-2-phenyl-N-(2,4,6-trimethoxy-phenyl)-acetamide

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a room temperature, stirred solution of 3-dodecyl-α-phenyl-5-isoxazole acetic acid and 5-dodecyl-α-phenyl-3-isoxazole acetic acid (48.42 g, 0.1303 mol) in dry tetrahydrofuran (1.4 L) was added in one portion 1,1'-carbonyldiimidazole (22.5 g, 0.139 mol), and the solution was stirred for 1.9 hours under nitrogen. To the mixture was added 2,4,6-trimethoxyaniline hydrochloride (28.5 g, 0.130 mol) and triethylamine (19 mL, 0.14 mol), and the mixture was stirred for 1.8 days under nitrogen. The mixture was rotoevaporated and partitioned between ethyl acetate and 1M HCl. The organic layer was washed (1M HCl; saturated NaCl), dried (MgSO4), and rotoevaporated to a tar. The tar was dissolved (THF) and repeatedly chromatographed on silica gel (230-400 mesh) using Heptane-ether-triethylaminemethanol (20:40:6:1) as eluent. Fractions containing pure compound were combined, rotoevaporated, dissolved in toluene, and reevaporated. The residue was crystallized from diisopropyl ether to give pure title compound; yield 17.6 g (25%); mp 107°-108° C.

후처리

  1. stirringthe mixture was stirred for 1.8 days under nitrogen
  2. custompartitioned between ethyl acetate and 1M HCl
  3. washThe organic layer was washed (1M HCl; saturated NaCl)
  4. dry with materialdried (MgSO4)
  5. dissolutionThe tar was dissolved (THF)
  6. customrepeatedly chromatographed on silica gel (230-400 mesh)
  7. additionFractions containing pure compound
  8. dissolutiondissolved in toluene
  9. customreevaporated
  10. customThe residue was crystallized from diisopropyl ether

출처 및 근거

ORD 기록
ord-21b20ba0a1d8458e9b13d24d39aab71f
출처 데이터셋
uspto-grants-1995_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05441975

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