Prolinamide, D- → 2-(Pyrrolidin-1-ylmethyl)pyrrolidine

HRID 232589

反応式

HRID 232589 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[NH:7]1[CH2:14][CH2:13][CH2:12][C@@H:8]1[C:9]([NH2:11])=O>O1CCCC1>[N:11]1([CH2:9][CH:8]2[CH2:12][CH2:13][CH2:14][NH:7]2)[CH2:13][CH2:12][CH2:8][CH2:9]1

参加物

4

反応物 2

HCID 447554Prolinamide, D-HCID 21226445Aluminium lithium hydride

生成物 1

HCID 1428252-(Pyrrolidin-1-ylmethyl)pyrrolidine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a suspension of 0.380 gm of lithium aluminum hydride in 15 ml of dry tetrahydrofuran is carefully added a solution of the D-proline amide (prepared in B above) in 10 ml tetrahydrofuran. The mixture is refluxed for 2 hrs then cooled and quenched with 2 ml of 2.5N sodium hydroxide. The mixture is filtered through a pad of sodium sulfate and the filter cake washed with 2×50 ml of ether. The combined filtrates are concentrated in vacuo to yield 0.80 gm of desired 2-(1-pyrrolidinylmethyl) pyrrolidine.

後処理

  1. temperatureThe mixture is refluxed for 2 hrs
  2. temperaturethen cooled
  3. customquenched with 2 ml of 2.5N sodium hydroxide
  4. filtrationThe mixture is filtered through a pad of sodium sulfate
  5. washthe filter cake washed with 2×50 ml of ether
  6. concentrationThe combined filtrates are concentrated in vacuo

出典と根拠

ORDレコード
ord-4420701b63bc47fd95512d4b562ec96d
出典データセット
uspto-grants-1997_01
特許番号
US05591737

関連ノート

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