Hydrochloric Acid → HCID 85405589, 화합물

HRID 1756745노트

반응식

HRID 1756745 반응식
[OH-].[K+].[N:3](OCCCC)=[O:4].[CH3:10][C:11]1[CH:27]=[CH:26][C:25]([CH3:28])=[CH:24][C:12]=1[O:13][CH2:14][C:15]1[CH:23]=[CH:22][CH:21]=[CH:20][C:16]=1[CH2:17][C:18]#[N:19].Cl>O.C1(C)C=CC=CC=1>[CH3:10][C:11]1[CH:27]=[CH:26][C:25]([CH3:28])=[CH:24][C:12]=1[O:13][CH2:14][C:15]1[CH:23]=[CH:22][CH:21]=[CH:20][C:16]=1[C:17]([C:18]#[N:19])=[N:3][OH:4]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 10996Butyl nitriteHCID 14797Potassium HydroxideHCID 11118528HCID 11118528, 화합물

생성물 1

HCID 85405589HCID 85405589, 화합물수율 92.8%

시약·촉매·용매 2

HCID 962Water용매HCID 1140Toluene용매

실험 절차

85% Potassium hydroxide (0.40 g, 6 mmol), toluene (5 ml) and butyl nitrite (0.62 g, 6 mmol) were added to 2-(2,5-dimethylphenoxymethyl)benzyl cyanide (1.26 g, 5 mmol). The mixture was stirred at room temperature for 8 hours. After completion of the reaction, water (100 ml) was added. The mixture was neutralized with hydrochloric acid, extracted with ether (100 ml), dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel chromatography (ethyl acetate/n-hexane) to give 2-(2,5-dimethylphenoxymethyl)-α-hydroxyiminobenzyl cyanide (1.30 g, Yield: 92.8%, E/Z=15/85).

후처리

  1. additionwas added
  2. extractionextracted with ether (100 ml)
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe resulting residue was purified by silica gel chromatography (ethyl acetate/n-hexane)

출처 및 근거

ORD 기록
ord-e26ecbd6c4454a98bf682cd71dea28c6
출처 데이터셋
uspto-grants-1995_08
특허 번호
US05442063

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