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

HRID 2388714
ノート
印刷プレビュー

反応式

HRID 2388714 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) is cooled to 0° C. At this temperature thionylchloride (7.54 ml, 104.3 mmol) is added slowly. The reaction mixture is heated to reflux for 12 h. The solvent is evaporated in vacuum. The residue is suspended in ethylacetate and is heated to reflux. The suspension is filtered while it is still hot. In the filtrate a white solid dropped out, which was filtered out and dried in vacuum to give Methyl 4-(piperidin-2-yl)butanoate hydrochloride (2) (3.49 g, 45%)

後処理

  1. temperatureThe reaction mixture is heated
  2. temperatureto reflux for 12 h
  3. customThe solvent is evaporated in vacuum
  4. temperatureis heated to reflux
  5. filtrationThe suspension is filtered while it
  6. additionIn the filtrate a white solid dropped out
  7. filtrationwhich was filtered out
  8. customdried in vacuum

出典と根拠

ORDレコード
ord-ad4ac774d20e456bbb3b96e11797832c
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08268814B2

反応ノート

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