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Potassium Carbonate → HCID 19041757、化合物

HRID 1684055
ノート
印刷プレビュー

反応式

HRID 1684055 の反応式
C(=O)([O-])[O-].[K+].[K+].[CH2:7](OS(C)(=O)=O)[CH:8]=[CH2:9].[O:15]1[C:19]2[CH:20]=[CH:21][C:22]([CH:24]3[CH:30]([CH3:31])[C:29]45[CH2:38][CH:26]([O:27][C:28]4=[CH:35][C:34](=[O:36])[C:33]([OH:37])=[CH:32]5)[CH2:25]3)=[CH:23][C:18]=2[O:17][CH2:16]1>CN(C=O)C.C(Cl)Cl>[O:15]1[C:19]2[CH:20]=[CH:21][C:22]([CH:24]3[CH:30]([CH3:31])[C:29]45[CH2:38][CH:26]([O:27][C:28]4=[CH:35][C:34](=[O:36])[C:33]([OH:37])=[C:32]5[CH2:9][CH:8]=[CH2:7])[CH2:25]3)=[CH:23][C:18]=2[O:17][CH2:16]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 812142-Propen-1-yl methanesulfonate2 回HCID 19041752HCID 19041752、化合物

生成物 1

HCID 19041757HCID 19041757、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

実験手順

Potassium carbonate (172.7 mg, 1.25 mmol) and mesyl allyl ether (113 mg, 0.83 mmol) are added to a stirred solution of 4-(1,3-benzodioxol-5-yl)-2,3,4,5-tetrahydro-7-hydroxy-5-methyl-8H-2,5a-methano-1-benzoxepin-8-one (109, as prepared in Example 54) in DMF (4 ml). The reaction is stirred at room temperature overnight, after which time TLC still shows unreacted starting material present. An additional 50 μl mesyl allyl ether is then added to the reaction and the reaction is then starred for another 24 hours. The reaction is diluted with methylene chloride and washed with 10% HCl followed by water. The extract is dried over sodium sulfate and concentrated in vacuo. The reaction is best purified by medium pressure liquid chromatography (MPLC) (i.e., flash chromatography on silica gel (25 g, 1:1 hexane-ethyl acetate as eluant) produces a contaminated product as determined by 1H NMR and flash chromatography on silica gel (30 g silica, 1:1:1 hexane-ethyl ether-methylene chloride) also produces a contaminated product as determined by 1H NMR). M+(CI)=367. 1H NMR: 0.64 (3H, d), 1.67 (1H, dd), 1.89 (1H, d), 2.06 (1H, m), 2.26 (2H, m), 2.49 (3H, m), 2.72 (1H, dd), 3.05 (1H, t), 5.08 (3H, m), 5.92 (2H, s), 6.15 (1H, s), 6.65 (3H, m).

後処理

  1. waitthe reaction is then starred for another 24 hours
  2. washwashed with 10% HCl
  3. dry with materialThe extract is dried over sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe reaction is best purified by medium pressure liquid chromatography (MPLC) (i.e., flash chromatography on silica gel (25 g, 1:1 hexane-ethyl acetate as eluant)
  6. customproduces a contaminated product
  7. customalso produces a contaminated product

出典と根拠

ORDレコード
ord-eb6190cfcc4e48e9a13ebdff6703a205
出典データセット
uspto-grants-1997_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05639782

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート