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Potassium Carbonate → (R)-1-(But-3-yn-1-yl)-2-methylpyrrolidine

HRID 2416135
ノート
印刷プレビュー

反応式

HRID 2416135 の反応式
C(=O)([O-])[O-].[K+].[K+].[C:7]([CH:10]([CH:12]([C:14](O)=O)O)O)(O)=O.[CH3:17][C@@H:18]1[CH2:22][CH2:21][CH2:20][NH:19]1.CC1C=CC(S(OCCC#C)(=O)=O)=CC=1.S(C1C=CC(C)=CC=1)([O-])(=O)=O>C(#N)C>[CH2:7]([N:19]1[CH2:20][CH2:21][CH2:22][C@H:18]1[CH3:17])[CH2:10][C:12]#[CH:14]
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 4

HCID 11430Potassium CarbonateHCID 85570p-ToluenesulfonateHCID 2720203-Butynyl p-toluenesulfonateHCID 23404464(2R)-2-Methylpyrrolidine tartrate

生成物 1

HCID 11367023(R)-1-(But-3-yn-1-yl)-2-methylpyrrolidine

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
85 °C

実験手順

A sealed pressure tube was charged potassium carbonate powder (18.4 g, 133.2 mmol, 325 mesh), milled (2R)-2-methylpyrrolidine tartrate (20.9 g, 88.8 mmol), 3-butynyl 4-methylbenzenesulfonate (15.7 mL, 88.8 mmol), and acetonitrile (105 mL). The mixture was heated at 85° C. and stirred for 16 hours. The completion of the reaction was monitored by gas chromatography until all the tosylate was consumed. The reaction mixture was cooled to room temperature, diluted with CH3CN (50 mL), and filtered. The filtrate was used in the next step without further purification. GC-MS m/z 138 (M+H)+.

後処理

  1. customwas consumed
  2. temperatureThe reaction mixture was cooled to room temperature
  3. additiondiluted with CH3CN (50 mL)
  4. filtrationfiltered
  5. customThe filtrate was used in the next step without further purification

出典と根拠

ORDレコード
ord-71e563b75b9d4fe6afb0f5c7fcaeb362
出典データセット
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06822101B2

反応ノート

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