Dimethylformamide → HCID 3839920, 화합물

HRID 1294097노트

반응식

HRID 1294097 반응식
[CH2:1]([O:3][C:4]1[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][C:5]=1[CH:6]=[O:7])[CH3:2].[CH2:13](Br)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.C(=O)([O-])[O-].[K+].[K+].CN(C)C=O>O>[CH2:13]([O:12][C:9]1[CH:10]=[CH:11][C:4]([O:3][CH2:1][CH3:2])=[C:5]([CH:8]=1)[CH:6]=[O:7])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 3572385HCID 3572385, 화합물

생성물 1

HCID 3839920HCID 3839920, 화합물수율 88.2%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
90 °C

실험 절차

A mixture of 2-ethoxy-5-hydroxybenzaldehyde (3.72 g), benzyl bromide (5.75 g), anhydrous potassium carbonate (3.10 g) and N,N-dimethylformamide (50 mL) was stirred at 90° C. for 3 hrs. The reaction mixture was poured into water and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated. The obtained residue was subjected to silica gel column chromatography to give crystals (5.06 g, 88%) of 5-benzyloxy-2-ethoxybenzaldehyde from a fraction eluted with ethyl acetate-hexane (1:4, v/v). Redrystallization from ethyl, acetate-hexane gave colorless prism crystals. melting point: 81-82° C.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-2ccfae50c58e4bb69850306fd79b324f
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07238716B2

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