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4-(3-Pyridylhydroxymethyl)phenol hydrochloride → 4-(3-Pyridylmethyl)phenol hydrochloride

HRID 2296050
ノート
印刷プレビュー

反応式

HRID 2296050 の反応式
[ClH:1].[N:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH:8](O)[C:9]2[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=2)[CH:3]=1>[Pd].C(O)(=O)C>[ClH:1].[N:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH2:8][C:9]2[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=2)[CH:3]=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 1

HCID 132901344-(3-Pyridylhydroxymethyl)phenol hydrochloride

生成物 1

HCID 132901364-(3-Pyridylmethyl)phenol hydrochloride収率 11.5%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒

実験手順

Under an atmosphere of hydrogen, a mixture of 1.9 g of the hydroxymethyl compound (prepared as described in Example 8), 1.0 g of 5% palladium on carbon and 12 ml of acetic acid was stirred at room temperature for 24 hours, and filtered. The filtrate was concentrated under reduced pressure. The residue was dissolved in water, neutralized with sodium bicarbonate, extracted with diethyl ether, and the extract was concentrated under reduced pressure. After addition of 6 N hydrochloric acid to the residue, the solution was concentrated under reduced pressure. The residue was purified by recrystallization from ethanol-diethyl ether to give 0.204 g of the title compound having the following physical characteristics:

後処理

  1. filtrationfiltered
  2. concentrationThe filtrate was concentrated under reduced pressure
  3. dissolutionThe residue was dissolved in water
  4. extractionextracted with diethyl ether
  5. concentrationthe extract was concentrated under reduced pressure
  6. additionAfter addition of 6 N hydrochloric acid to the residue
  7. concentrationthe solution was concentrated under reduced pressure
  8. customThe residue was purified by recrystallization from ethanol-diethyl ether

出典と根拠

ORDレコード
ord-21bf4e099ff44c5c93caf948552c110c
出典データセット
uspto-grants-1984_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04427682

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート