Potassium Carbonate → HCID 18333474、化合物

HRID 1683095

反応式

HRID 1683095 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2([CH2:14][CH2:15][CH2:16][O:17][CH:18]3[CH2:23][CH2:22][CH2:21][CH2:20][O:19]3)[CH2:13][NH:12][CH2:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8].C([O-])([O-])=O.[K+].[K+].[CH3:30][O:31][C:32]1[CH:33]=[C:34]([CH:37]=[C:38]([O:42][CH3:43])[C:39]=1[O:40][CH3:41])[CH2:35]Br>C1COCC1.O.C(OCC)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2([CH2:14][CH2:15][CH2:16][O:17][CH:18]3[CH2:23][CH2:22][CH2:21][CH2:20][O:19]3)[CH2:13][N:12]([CH2:35][C:34]3[CH:37]=[C:38]([O:42][CH3:43])[C:39]([O:40][CH3:41])=[C:32]([O:31][CH3:30])[CH:33]=3)[CH2:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8]

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 103552715-(Bromomethyl)-1,2,3-trimethoxybenzeneHCID 183334184-(3,4-Dichloro-phenyl)-4-[3-(tetrahydro-pyran-2-yloxy)-propyl]-pyrrolidine

生成物 1

HCID 18333474HCID 18333474、化合物

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 21881883Oxolane--water (1/1)溶媒

実験手順

Combine 4-(3,4-dichloro-phenyl)-4-[3-(tetrahydro-pyran-2-yloxy)-propyl]-pyrrolidine (10 mmol), K2CO3 (30 mmol), and 3,4,5-trimethoxy-benzyl bromide (10 mmol) in THF/H2O (4/1, 200 mL). Heat to reflux and stir for 16 h. Concentrate in vacuo to obtain a residue. Dilute the residue with ethyl acetate and extract with H2O. Separate the layers, dry the organic layer over MgSO4, filter, and concentrate in vacuo. Chromatograph on silica gel to give the title compound.

後処理

  1. temperatureHeat
  2. temperatureto reflux
  3. concentrationConcentrate in vacuo
  4. customto obtain a residue
  5. extractionextract with H2O
  6. customSeparate the layers
  7. dry with materialdry the organic layer over MgSO4
  8. filtrationfilter
  9. concentrationconcentrate in vacuo

出典と根拠

ORDレコード
ord-2675bd1e05694375a2bb9842c49604f0
出典データセット
uspto-grants-1997_06
特許番号
US05635510

関連ノート

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