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Nanofin → HCID 13277417、化合物

HRID 1075853
ノート
印刷プレビュー

反応式

HRID 1075853 の反応式
[Cl:1][CH2:2][CH:3]([OH:18])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[CH2:12][C:13]1[S:14][CH:15]=[CH:16][CH:17]=1.[CH3:19][CH:20]1[CH2:25][CH2:24][CH2:23][CH:22]([CH3:26])[NH:21]1>C(O)C>[ClH:1].[CH3:19][CH:20]1[CH2:25][CH2:24][CH2:23][CH:22]([CH3:26])[N:21]1[CH2:2][CH:3]([OH:18])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[CH2:12][C:13]1[S:14][CH:15]=[CH:16][CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 68843NanofinHCID 21541296HCID 21541296、化合物

生成物 1

HCID 13277417HCID 13277417、化合物収率 53.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 2.8 g of 1-chloro-3[2-(2-thienylmethyl)phenoxy]-2-propanol, 2.3 g of 2,6-dimethylpiperidine in 30 ml of ethanol is refluxed for 15 hours. The ethanol is then removed, and the residue is dissolved in ether. The insoluble matter is filtered off, and the filtrated is extracted with two 50 ml portions of 10% hydrochloric acid. The aqueous layer is made alkaline with sodium hydroxide, and separated oil is extracted with ether. The ether layer is dried over anhydrous potassium carbonate, and the solvent is removed. The residue (crude product) is purified by column chromatography and converted into the hydrochloride in the same manner as in above method (a) to give 2.1 g of 1-(2,6-dimethylpiperidino)-3-[2-(2-thienylmethyl)phenoxy]-2-propanol hydrochloride as colorless crystals, melting at 152°-153°C.

後処理

  1. customThe ethanol is then removed
  2. dissolutionthe residue is dissolved in ether
  3. filtrationThe insoluble matter is filtered off
  4. extractionthe filtrated is extracted with two 50 ml portions of 10% hydrochloric acid
  5. customseparated oil
  6. extractionis extracted with ether
  7. dry with materialThe ether layer is dried over anhydrous potassium carbonate
  8. customthe solvent is removed
  9. customThe residue (crude product) is purified by column chromatography

出典と根拠

ORDレコード
ord-f2b48cea1309470eb860e7313c36445d
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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