Ethyl Acetate → 4-Morpholinobenzaldehyde

HRID 32824

반응식

HRID 32824 반응식
[O:1]1CCO[CH:2]1[C:6]1[CH:11]=[CH:10][C:9]([N:12]2[CH2:17][CH2:16][O:15][CH2:14][CH2:13]2)=[CH:8][CH:7]=1.C(OCC)(=O)C>CO.Cl.O>[N:12]1([C:9]2[CH:8]=[CH:7][C:6]([CH:2]=[O:1])=[CH:11][CH:10]=2)[CH2:17][CH2:16][O:15][CH2:14][CH2:13]1

참가 물질

6

반응물 2

HCID 8857Ethyl AcetateHCID 691435844-(4-[1,3]Dioxolan-2-yl-phenyl)-morpholine

생성물 1

HCID 2913494-Morpholinobenzaldehyde

시약·촉매·용매 3

HCID 313Hydrochloric Acid촉매HCID 962Water촉매HCID 887Methanol용매

실험 절차

A mixture of 4-(4-[1,3]dioxolan-2-yl-phenyl)-morpholine (690 mg, 2.933 mmol) in methanol (5 mL) was treated with 10 drops concentrated aqueous hydrochloric acid. The mixture was stirred at room temperature for 1 hour. To this solution was added 5 drops of water and stirring was continued for 2 hours at ambient temperature. The solution was then poured into ethyl acetate (50 mL) and washed with saturated aqueous sodium bicarbonate (2×50 mL) and extracted with ethyl acetate (2×50 mL). The combined organic extracts were dried over sodium sulfate, filtered and concentrated to give 4-morpholin-4-yl-benzaldehyde as a tan waxy solid (550 mg, 98%).

후처리

  1. stirringstirring
  2. waitwas continued for 2 hours at ambient temperature
  3. washwashed with saturated aqueous sodium bicarbonate (2×50 mL)
  4. extractionextracted with ethyl acetate (2×50 mL)
  5. dry with materialThe combined organic extracts were dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-a0b4f1a6848b4f2d807fa2206b9e18b4
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07427635B2

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