Tetrahydrofuran → (1-(Pyrrolidin-1-yl)cyclopropyl)methanol

HRID 496069ノート

反応式

HRID 496069 の反応式
[N:1]1([C:6]2([C:9](OCC)=[O:10])[CH2:8][CH2:7]2)[CH2:5][CH2:4][CH2:3][CH2:2]1.O1CCCC1.[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[Na+]>O>[N:1]1([C:6]2([CH2:9][OH:10])[CH2:8][CH2:7]2)[CH2:5][CH2:4][CH2:3][CH2:2]1

参加物

6

反応物 4

HCID 8028Tetrahydrofuran2 回HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 22325082HCID 22325082、化合物

生成物 1

HCID 22325087(1-(Pyrrolidin-1-yl)cyclopropyl)methanol

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

20.5 g of the product obtained in Step 3 and 100 ml of tetrahydrofuran are poured, over 5 minutes, into a suspension containing 8.57 g of lithium aluminium hydride and 400 ml of tetrahydrofuran. The mixture is heated at reflux for 2 hours, cooled to 5° C. and hydrolysed by successive additions of 9 ml of water, 9 ml of 4N sodium hydroxide solution and then 27 ml of water. The aluminium compound is filtered off and rinsed with tetrahydroflran. The combined filtrates are concentrated to dryness, allowing the desired product to be obtained (liquid).

後処理

  1. temperatureThe mixture is heated
  2. temperatureat reflux for 2 hours
  3. filtrationThe aluminium compound is filtered off
  4. washrinsed with tetrahydroflran
  5. concentrationThe combined filtrates are concentrated to dryness
  6. customto be obtained (liquid)

出典と根拠

ORDレコード
ord-9fa619de0f9a40589588bee84f4458b7
出典データセット
uspto-grants-2005_09
特許番号
US06943184B2

反応ノート

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