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Methanol → Methyl 4-(piperidin-2-yl)butanoate hydrochloride

HRID 1881683
ノート
印刷プレビュー

反応式

HRID 1881683 の反応式
Cl.[NH:2]1[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]1[CH2:8][CH2:9][CH2:10][C:11]([OH:13])=[O:12].S(Cl)([Cl:16])=O.[CH3:18]O>>[ClH:16].[NH:2]1[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]1[CH2:8][CH2:9][CH2:10][C:11]([O:13][CH3:18])=[O:12]
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 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 124163274-(Piperidin-2-yl)butanoic acid--hydrogen chloride (1/1)

生成物 1

HCID 66772062Methyl 4-(piperidin-2-yl)butanoate hydrochloride収率 45%

実験手順

A solution of 4-(2-piperidinyl)butanoic acid hydrochloride (5.95 g, 34.8 mmol) in methanol (104 ml) was cooled to 0° C. Thionyl chloride (7.54 ml, 104.3 mmol) was slowly added at this temperature. The reaction mixture was heated under reflux for 12 h. The solvent was evaporated off under reduced pressure. The residue was suspended in ethyl acetate and the suspension was heated under reflux. The suspension was filtered hot. A white precipitate precipitates out in the filtrate, and was filtered out and dried under reduced pressure to give the product methyl 4-(piperidine-2-yl)butanoate hydrochloride (2) (3.49 g, 45%).

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureunder reflux for 12 h
  3. customThe solvent was evaporated off under reduced pressure
  4. temperaturethe suspension was heated
  5. temperatureunder reflux
  6. filtrationThe suspension was filtered hot
  7. customA white precipitate precipitates out in the filtrate
  8. filtrationwas filtered out
  9. customdried under reduced pressure

出典と根拠

ORDレコード
ord-1bfeece9c79545f4ba90cda4d6079ccd
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08318769B2

反応ノート

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