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Methanol → 2-Piperidineacetic acid ethyl ester hydrochloride

HRID 1881678
ノート
印刷プレビュー

反応式

HRID 1881678 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][C:8]([O:10][CH2:11][CH3:12])=[O:9].C(Cl)(Cl)[Cl:14].CO>C(O)C.O=[Pt]=O>[ClH:14].[NH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[CH2:7][C:8]([O:10][CH2:11][CH3:12])=[O:9]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 887MethanolHCID 6212Chloroform2 回HCID 75960Ethyl 2-pyridylacetate

生成物 1

HCID 242012202-Piperidineacetic acid ethyl ester hydrochloride

試薬・触媒・溶媒 2

HCID 345198Adams' catalyst触媒HCID 702Ethanol溶媒

反応条件

温度
40 °C

実験手順

Ethyl 2-(pyridin-2-yl)acetate (24.51 g, 148.4 mmol) was dissolved in ethanol (130 ml), and PtO2 (3.37 g, 14.84 mmol, 0.1 eq.) and chloroform (20 ml) were added. The suspension was stirred under an H2 atmosphere (8 bar) at 40° C. overnight. According to TLC control (silica gel, MC/methanol 95:5), the reaction was not complete, so that further chloroform (15 ml) was added and the mixture was stirred under an H2 atmosphere (8 bar) at 40° C. for a further 2 d (TLC control). After cooling, the catalyst was first removed by filtering over filtering earth and the filtrate was concentrated to dryness in vacuo. The ethyl 2-(piperidin-2-yl)acetate hydrochloride was employed in the next stage without further purification.

後処理

  1. stirringthe mixture was stirred under an H2 atmosphere (8 bar) at 40° C. for a further 2 d (TLC control)
  2. temperatureAfter cooling
  3. customthe catalyst was first removed
  4. filtrationby filtering
  5. filtrationover filtering earth
  6. concentrationthe filtrate was concentrated to dryness in vacuo
  7. customThe ethyl 2-(piperidin-2-yl)acetate hydrochloride was employed in the next stage without further purification

出典と根拠

ORDレコード
ord-7701260652c740b399edc0f3d0b34a14
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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