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Tetrahydrofuran toluene → HCID 178472330, 화합물

HRID 2368131
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HRID 2368131 반응식
C1(COC2C=CC3C=[C:11]([C@H:13]4[CH2:18][CH2:17][C@H:16]([O:19][CH2:20][C:21](N5CCOCC5)=[O:22])[CH2:15][CH2:14]4)[O:12]C=3C=2)CC1.[CH3:31][Mg]Br.[C:34]1([CH3:40])[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1.[CH2:41]1[CH2:45][O:44][CH2:43][CH2:42]1>C1COCC1>[CH:41]1([CH2:45][O:44][C:37]2[CH:38]=[CH:39][C:34]3[CH:40]=[C:11]([C@H:13]4[CH2:14][CH2:15][C@H:16]([O:19][CH2:20][C:21](=[O:22])[CH3:31])[CH2:17][CH2:18]4)[O:12][C:35]=3[CH:36]=2)[CH2:42][CH2:43]1
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참가 물질

5

반응물 3

HCID 22635083Tetrahydrofuran tolueneHCID 178418573HCID 178418573, 화합물HCID 178521450HCID 178521450, 화합물

생성물 1

HCID 178472330HCID 178472330, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

To a solution of 4-[({trans-4-[6-(cyclopropylmethoxy)-1-benzofuran-2-yl]cyclohexyl}oxy)acetyl]morpholine (881 mg) in THF (10 mL) was added a solution (1.5 M, 2.84 mL) of methylmagnesium bromide in toluene/THF under ice-cooling. The mixture was stirred at 0° C. for 1 hr and extracted with ethyl acetate and 1M hydrochloric acid. The obtained organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel chromatography (hexane/ethyl acetate) to give the title compound (556 mg).

후처리

  1. temperaturecooling
  2. extractionextracted with ethyl acetate and 1M hydrochloric acid
  3. washThe obtained organic layer was washed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe obtained residue was purified by silica gel chromatography (hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-f315c2fe6a004c1a9ecb134f34e83d81
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08703758B2

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