Methyl iodide → benzyl N-(4-iodophenyl)-N-methylcarbamate

HRID 1018006

반응식

HRID 1018006 반응식
[CH2:1]([O:8][C:9]([NH:11][C:12]1[CH:17]=[CH:16][C:15]([I:18])=[CH:14][CH:13]=1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Na+].[CH3:21]I>CN(C)C=O>[CH2:1]([O:8][C:9]([N:11]([CH3:21])[C:12]1[CH:13]=[CH:14][C:15]([I:18])=[CH:16][CH:17]=1)=[O:10])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 1245679N-Cbz-4-iodoaniline

생성물 1

HCID 18404743benzyl N-(4-iodophenyl)-N-methylcarbamate수율 96.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A stirred solution of N-benzyloxycarbonyl-4-iodoaniline (11.5 g, Reference Example 27) in dimethylformamide (70 ml) was treated portionwise with sodium hydride (⅙ g of a 60% dispersion in oil), under nitrogen and at room temperature. When effervescence had ceased methyl iodide (6.3 g) was added and the mixture was stirred at room temperature for 2 hours, after which it was partitioned between ethyl acetate and water. The organic phase was separated, then dried over magnesium sulphate and then evaporated to give the title compound (11.5 g) as a pink oil.

후처리

  1. customat room temperature
  2. additionwas added
  3. customafter which it was partitioned between ethyl acetate and water
  4. customThe organic phase was separated
  5. dry with materialdried over magnesium sulphate
  6. customevaporated

출처 및 근거

ORD 기록
ord-da2c498bf9dc44d797f26ef8ea60d3f8
출처 데이터셋
uspto-grants-2002_11
특허 번호
US06479519B1

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