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Potassium Carbonate → 4-((S)-2-Methyl-pyrrolidin-1-yl)-butyric acid ethyl ester

HRID 1695228
ノート
印刷プレビュー

反応式

HRID 1695228 の反応式
Cl.[CH3:2][C@H:3]1[CH2:7][CH2:6][CH2:5][NH:4]1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:15][CH2:16][CH2:17][C:18]([O:20][CH2:21][CH3:22])=[O:19]>CC(=O)CC>[CH2:21]([O:20][C:18](=[O:19])[CH2:17][CH2:16][CH2:15][N:4]1[CH2:5][CH2:6][CH2:7][C@@H:3]1[CH3:2])[CH3:22]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 76300Ethyl 4-bromobutyrateHCID 44891221(2S)-2-Methylpyrrolidine--hydrogen chloride (1/1)

生成物 1

HCID 672744374-((S)-2-Methyl-pyrrolidin-1-yl)-butyric acid ethyl ester収率 100.4%

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

(S)-2-methyl-pyrrolidine hydrochloride (0.8 g, 6.6 mmol, 1.1 eq) was dissolved in 2-butanone (20 mL) and potassium carbonate (1.7 g, 12.6 mmol, 2.1 eq) was added. Ethyl 4-bromobutyrate (0.86 mL, 6.0 mmol, 1.0 eq) was added and the reaction mixture was refluxed for 2 days. The mixture was allowed to cool to room temperature and any solid present was filtered off and washed with ether. The filtrate was concentrated under reduced pressure to give 1.20 g of the title compound (yield 99%) which was used in the next step without further purification.

後処理

  1. temperaturethe reaction mixture was refluxed for 2 days
  2. filtrationany solid present was filtered off
  3. washwashed with ether
  4. concentrationThe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-ab5d76ef0eb847e68ad76a30413dd75f
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08163729B2

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