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Potassium Carbonate → HCID 21541283, 화합물

HRID 1075852
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HRID 1075852 반응식
Cl[CH2:2][CH:3]([OH:13])[CH2:4][N:5]1[CH:10]([CH3:11])[CH2:9][CH2:8][CH2:7][CH:6]1[CH3:12].[CH3:14][O:15][CH2:16][CH2:17][O:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=1[OH:25].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH3:12][CH:6]1[CH2:7][CH2:8][CH2:9][CH:10]([CH3:11])[N:5]1[CH2:4][CH:3]([OH:13])[CH2:2][O:25][C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=1[O:18][CH2:17][CH2:16][O:15][CH3:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 112752342-(2-Methoxyethoxy)phenolHCID 20373484HCID 20373484, 화합물

생성물 1

HCID 21541283HCID 21541283, 화합물수율 67.4%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

4.5 g of 1-chloro-3-(2,6-dimethylpiperidino)-2-propanol is added to a mixture of 3.4 g of 2-(2-methoxyethoxy)phenol, 2.8 g of anhydrous potassium carbonate and 70 ml of acetone, and the resulting mixture is refluxed with stirring for 20 hours. The insoluble matter is then filtered off, and the filtrate is concentrated under reduced pressure. To the residue is added ether, and the ethereal solution is extracted with two 80 ml portions of 10% hydrochloric acid. The aqueous layer is made alkaline with sodium hyroxide, and the separated oil is extracted twice with ether. The ether layer is dried over anhydrous potassium carbonate, and the ether is removed to give 4.6 g of 1-(2,6-dimethylpiperidino)-3-[2-(2-methoxyethoxy)phenoxy]-2-propanol, melting at 92°-94°C.

후처리

  1. temperaturethe resulting mixture is refluxed
  2. filtrationThe insoluble matter is then filtered off
  3. concentrationthe filtrate is concentrated under reduced pressure
  4. additionTo the residue is added ether
  5. extractionthe ethereal solution is extracted with two 80 ml portions of 10% hydrochloric acid
  6. extractionthe separated oil is extracted twice with ether
  7. dry with materialThe ether layer is dried over anhydrous potassium carbonate
  8. customthe ether is removed

출처 및 근거

ORD 기록
ord-f4a549da3bae419ba979821121690a7e
출처 데이터셋
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03954776

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