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Methyl iodide → HCID 178501764、化合物

HRID 2225610
ノート
印刷プレビュー

反応式

HRID 2225610 の反応式
[CH:1](N(C(C)C)CC)(C)C.IC.[CH3:12][C@H:13]1[CH2:18][CH2:17][C@H:16]([NH:19][C:20](=[O:36])[CH:21]=[CH:22][C:23]2[CH:28]=[CH:27][C:26]([O:29][CH2:30][C:31]([OH:33])=[O:32])=[C:25]([O:34][CH3:35])[CH:24]=2)[CH2:15][CH2:14]1>C(Cl)Cl>[CH3:12][C@H:13]1[CH2:14][CH2:15][C@H:16]([NH:19][C:20](=[O:36])[CH:21]=[CH:22][C:23]2[CH:28]=[CH:27][C:26]([O:29][CH2:30][C:31]([O:33][CH3:1])=[O:32])=[C:25]([O:34][CH3:35])[CH:24]=2)[CH2:17][CH2:18]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 81531DiisopropylethylamineHCID 178490558HCID 178490558、化合物

生成物 1

HCID 178501764HCID 178501764、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

30 ml of diisopropylethylamine and 1.0 ml of iodomethane were added to a solution of 1.84 g of N-(trans-4-methylcyclohexyl)-4-(carboxymethoxy)-3-methoxycinnamamide (Example 172) in 50 ml methylene chloride. The solution was stirred for 16 hours, while it was refluxed. After reaction, the reaction solution was washed three times with 200 ml of an aqueous sodium thiosulfate solution and once with an aqueous sodium chloride solution, and was dried over magnesium sulfate. Then, the solvent was removed in vacuo. The product obtained was recrystallized from methylene chloride/ether, yielding 1.38 g of N-(trans-4-methylcyclohexyl)4-(methoxycarbonylmethoxy)-3-methoxycinnamamide (a compound of the present invention) as white crystal, which had the following physiochemical properties:

後処理

  1. temperaturewas refluxed
  2. customAfter reaction
  3. washthe reaction solution was washed three times with 200 ml of an aqueous sodium thiosulfate solution
  4. dry with materialonce with an aqueous sodium chloride solution, and was dried over magnesium sulfate
  5. customThen, the solvent was removed in vacuo
  6. customThe product obtained
  7. customwas recrystallized from methylene chloride/ether

出典と根拠

ORDレコード
ord-5d7a243dde064344a937b21c0c09833f
出典データセット
uspto-grants-1994_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05344845

反応ノート

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