Ethyl Acetate → 5-[4-(2-Azepan-1-yl-ethoxy)-phenyl]-5-methyl-5,11-dihydro-chromeno[4,3-c]chromene-2,8-diol

HRID 2214299노트

반응식

HRID 2214299 반응식
C([Si](C)(C)[O:6][C:7]1[CH:8]=[CH:9][C:10]2[C:11]3[C:24]([C:26]4[CH:41]=[CH:40][C:29]([O:30][CH2:31][CH2:32][N:33]5[CH2:39][CH2:38][CH2:37][CH2:36][CH2:35][CH2:34]5)=[CH:28][CH:27]=4)([CH3:25])[O:23][C:22]4[CH:21]=[C:20]([O:42][Si](C(C)(C)C)(C)C)[CH:19]=[CH:18][C:17]=4[C:12]=3[CH2:13][O:14][C:15]=2[CH:16]=1)(C)(C)C.[F-].C([N+](CCCC)(CCCC)CCCC)CCC.[NH4+].[Cl-].C(OCC)(=O)C>C1COCC1>[N:33]1([CH2:32][CH2:31][O:30][C:29]2[CH:28]=[CH:27][C:26]([C:24]3([CH3:25])[C:11]4[C:10]5[CH:9]=[CH:8][C:7]([OH:6])=[CH:16][C:15]=5[O:14][CH2:13][C:12]=4[C:17]4[CH:18]=[CH:19][C:20]([OH:42])=[CH:21][C:22]=4[O:23]3)=[CH:41][CH:40]=2)[CH2:39][CH2:38][CH2:37][CH2:36][CH2:35][CH2:34]1

참가 물질

6

반응물 4

HCID 8857Ethyl AcetateHCID 25517Ammonium ChlorideHCID 2724141Tetrabutylammonium FluorideHCID 219592481-(2-{4-[2,8-Bis-(tert-butyl-dimethyl-silyloxy)-5-methyl-5,11-dihydro-chromeno[4,3-c]chromen-5-yl]-phenoxy}-ethyl)-azepane

생성물 1

HCID 219592555-[4-(2-Azepan-1-yl-ethoxy)-phenyl]-5-methyl-5,11-dihydro-chromeno[4,3-c]chromene-2,8-diol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 1-(2-{4-[2,8-bis-(tert-butyl-dimethyl-silyloxy)-5-methyl-5,11-dihydro-chromeno[4,3-c]chromen-5-yl]-phenoxy}-ethyl)-azepane (77.5 mg, 0.11 mmol) in THF (7 mL) was added tetrabutylammonium fluoride (1M in THF, 213 μL, 0.21 mmol). The mixture was stirred at room temperature for 40 min. Saturated NH4Cl was then added followed by addition of ethyl acetate. The resulting layers were separated, organic layer was washed with brine, and dried over MgSO4. The remaining solvent was evaporated and the residue dried under vacuum for 2 h at room temperature to yield the title compound, which was carried on to the next step without further purification.

후처리

  1. customThe resulting layers were separated
  2. washorganic layer was washed with brine
  3. dry with materialdried over MgSO4
  4. customThe remaining solvent was evaporated
  5. customthe residue dried under vacuum for 2 h at room temperature

출처 및 근거

ORD 기록
ord-fecd757a7e2949669e3879b722d827e3
출처 데이터셋
uspto-grants-2006_09
특허 번호
US07105679B2

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