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Potassium Carbonate → HCID 21541283、化合物

HRID 1075852
ノート
印刷プレビュー

反応式

HRID 1075852 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 112752342-(2-Methoxyethoxy)phenolHCID 20373484HCID 20373484、化合物

生成物 1

HCID 21541283HCID 21541283、化合物収率 67.4%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f4a549da3bae419ba979821121690a7e
出典データセット
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03954776

反応ノート

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