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

HRID 2214299ノート

反応式

HRID 2214299 の反応式
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

参加物

6

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-fecd757a7e2949669e3879b722d827e3
出典データセット
uspto-grants-2006_09
特許番号
US07105679B2

反応ノート

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