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Methyl iodide → HCID 178501764, 화합물

HRID 2225610
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HRID 2225610 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 81531DiisopropylethylamineHCID 178490558HCID 178490558, 화합물

생성물 1

HCID 178501764HCID 178501764, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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:

후처리

  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

출처 및 근거

ORD 기록
ord-5d7a243dde064344a937b21c0c09833f
출처 데이터셋
uspto-grants-1994_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05344845

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