Ethanol → 3-(7,8-dimethoxy-2-oxo-1,2-dihydro-3H-benzo[d]azepin-3-yl)propanal

HRID 1380866

반응식

HRID 1380866 반응식
C([O:3][CH:4](OCC)[CH2:5][CH2:6][N:7]1[C:13](=[O:14])[CH2:12][C:11]2[CH:15]=[C:16]([O:21][CH3:22])[C:17]([O:19][CH3:20])=[CH:18][C:10]=2[CH:9]=[CH:8]1)C.C(O)C>S(=O)(=O)(O)O>[CH3:20][O:19][C:17]1[C:16]([O:21][CH3:22])=[CH:15][C:11]2[CH2:12][C:13](=[O:14])[N:7]([CH2:6][CH2:5][CH:4]=[O:3])[CH:8]=[CH:9][C:10]=2[CH:18]=1

참가 물질

4

반응물 2

HCID 702EthanolHCID 135796433-(7,8-Dimethoxy-1,3-dihydro-2H-3-benzazepin-2-on-3-yl)-propionaldehyde diethylacetal

생성물 1

HCID 135796613-(7,8-dimethoxy-2-oxo-1,2-dihydro-3H-benzo[d]azepin-3-yl)propanal

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

First, 3-(7,8-Dimethoxy-1,3-dihydro-2H-3-benzazepin-2-on-3-yl)-propionaldehyde diethyl acetal (3.5 g, 0.01 mol) is heated in 2N sulphuric acid (50 ml) and ethanol (50 ml) to 40° C. for 2 hours. The alcohol is then distilled off in vacuo, the residue is made alkaline with saturated potassium carbonate solution with cooling and extracted several times with ethyl acetate. The ethyl acetate extract is extracted twice with sodium hydrogensulphite solution. The bisulphite extract is acidified with concentrated hydrochloric acid and heated for half an hour to 40° C. in vacuo in order to eliminate the sulphur dioxide. Then, saturated potassium carbonate solution is added and the mixture is extracted several times with methylene chloride, dried over magnesium sulphate and evaporated. Yield: 1.7 g. Mp: 95°-96° C.

후처리

  1. distillationThe alcohol is then distilled off in vacuo
  2. temperaturewith cooling
  3. extractionextracted several times with ethyl acetate
  4. extractionThe ethyl acetate extract
  5. extractionis extracted twice with sodium hydrogensulphite solution
  6. extractionThe bisulphite extract
  7. temperatureheated for half an hour to 40° C. in vacuo in order
  8. additionThen, saturated potassium carbonate solution is added
  9. extractionthe mixture is extracted several times with methylene chloride
  10. dry with materialdried over magnesium sulphate
  11. customevaporated

출처 및 근거

ORD 기록
ord-7c522c6de0974f9ea436431392b948db
출처 데이터셋
uspto-grants-1986_04
특허 번호
US04584293

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