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Methyl iodide → HCID 53922683, 화합물

HRID 1418362
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HRID 1418362 반응식
[C:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[NH:9][C:10](=[O:15])[C:11]([F:14])([F:13])[F:12])#[N:2].[H-].[Na+].[CH3:18]I>C1COCC1>[C:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]([CH3:18])[C:10](=[O:15])[C:11]([F:13])([F:12])[F:14])#[N:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 9203669HCID 9203669, 화합물

생성물 1

HCID 53922683HCID 53922683, 화합물수율 93.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

N-(2-Cyanophenyl)-2,2,2-trifluoroacetamide (3 g, 0.014 mol) was added to sodium hydride (60% in oil, 0.62 g, 0.026 mol) in THF (40 ml) under nitrogen and stirred for 4 h. Methyl iodide (8.7 ml, 0.14 mol) was added and stirring continued overnight. The mixture was poured onto brine and extracted with ethyl acetate, dried over sodium sulphate and evaporated to give the product (3 g), MS (+EI) 228 (M+). 1H NMR (CDCl3) 7.8 (1H, d), 7.7 (1H, dd), 7.4 (1H, dd), 7.4 (1H, d), 3.43 (3H, s).

후처리

  1. stirringstirring continued overnight
  2. additionThe mixture was poured onto brine
  3. extractionextracted with ethyl acetate
  4. dry with materialdried over sodium sulphate
  5. customevaporated

출처 및 근거

ORD 기록
ord-d4847f0527ba4fe6a942a99e84acd3b8
출처 데이터셋
uspto-grants-1999_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05883102

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