Potassium Carbonate → HCID 20239573, 화합물

HRID 364651

반응식

HRID 364651 반응식
[CH3:1][O:2][C:3]1[CH:19]=[CH:18][CH:17]=[CH:16][C:4]=1[C:5]([CH2:14][CH3:15])([OH:13])[C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][CH:7]=1.C(=O)([O-])[O-].[K+].[K+].[OH-].[CH2:27]([N+:31](CCCC)([CH2:36][CH2:37]CC)[CH2:32][CH2:33]CC)[CH2:28][CH2:29]C.Cl.C(N(CC)CCCCl)C>C(C(C)=O)C(C)C>[CH3:1][O:2][C:3]1[CH:19]=[CH:18][CH:17]=[CH:16][C:4]=1[C:5]([CH2:14][CH3:15])([OH:13])[C:6]1[CH:11]=[CH:10][C:9]([O:12][CH2:29][CH2:28][CH2:27][N:31]([CH2:36][CH3:37])[CH2:32][CH3:33])=[CH:8][CH:7]=1

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 145749Diethylaminopropyl chloride, hydrochlorideHCID 2723671Tetrabutylammonium HydroxideHCID 14727321HCID 14727321, 화합물

생성물 1

HCID 20239573HCID 20239573, 화합물

시약·촉매·용매 1

HCID 7909Methyl Isobutyl Ketone용매

실험 절차

12.9 g. of 2-methoxy-4'-hydroxy-α-ethyl-benzhydrol are dissolved in 100 ml. of methyl isobutyl ketone, 23 g. of anhydrous potassium carbonate 0.4 ml. of a 40% tetrabutyl ammoniumhydroxide solution and 10.3 g. of 3-diethylamino-propyl chloride hydrochloride are added, and the solution is heated up to the boiling point. The reaction mixture is boiled for 4 hours, and the solvent is distilled off under reduced pressure. To the residue water is added, and it is extracted with benzene. The benzene phase is washed with a 5% potassium hydroxide solution and subsequently with water. After drying over anhydrous potassium carbonate, benzene is distilled off under reduced pressure, and the residue is fractionated in vacuo to yield 13.2 g. of the title compound, boiling at 200° to 203° C./13.3 Pa.

후처리

  1. temperaturethe solution is heated up to the boiling point
  2. distillationthe solvent is distilled off under reduced pressure
  3. additionTo the residue water is added
  4. extractionit is extracted with benzene
  5. washThe benzene phase is washed with a 5% potassium hydroxide solution and subsequently with water
  6. dry with materialAfter drying over anhydrous potassium carbonate, benzene
  7. distillationis distilled off under reduced pressure
  8. customto yield 13.2 g

출처 및 근거

ORD 기록
ord-e0b56837ae5643779e5db1a46ccc4680
출처 데이터셋
uspto-grants-1986_08
특허 번호
US04605672

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