Water → HCID 18357786, 화합물

HRID 427991노트

반응식

HRID 427991 반응식
[CH3:1][C:2]1[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][C:3]=1[O:4][CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[CH2:12][C:13]#[N:14].[H-].[Na+].[CH2:22](I)[CH3:23].O>CN(C)C=O>[CH3:1][C:2]1[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][C:3]=1[O:4][CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[CH:12]([CH2:22][CH3:23])[C:13]#[N:14]

참가 물질

6

반응물 4

HCID 962WaterHCID 6340IodoethaneHCID 24758Sodium hydrideHCID 11118528HCID 11118528, 화합물

생성물 1

HCID 18357786HCID 18357786, 화합물수율 86%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 2-[2-(2,5-dimethylphenoxymethyl)phenyl]acetonitrile (2.00 g, 8.0 mmol) in N,N-dimethylformamide (20 ml) was stirred at 0° C. 60% oily sodium hydride (0.38 g, 9.5 mmol) was added thereto, and then ethyl iodide (1.37 g, 8.8 mmol) was added dropwise over 5 minutes. After 1 hour, water was added, and the mixture was extracted with ethyl acetate, washed successively with water and saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated, and the residue was purified by column chromatography on silica gel (n-hexane/ethyl acetate=19/1) to give the desired compound 2-[2-(2,5-dimethylphenoxymethyl)phenyl]butyronitrile (1.91 g, 86%) as an oil.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washwashed successively with water and saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated
  5. customthe residue was purified by column chromatography on silica gel (n-hexane/ethyl acetate=19/1)

출처 및 근거

ORD 기록
ord-39bcea21a3454ab79de60da95db07310
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06313150B1

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