Water → 3-Aminomethyl-1-benzhydrylazetidine

HRID 622550ノート

反応式

HRID 622550 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]([CH:9]1[CH2:12][N:11]([CH:13]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH2:10]1)#[N:8].O.[OH-].[Na+]>O1CCCC1>[C:14]1([CH:13]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[N:11]2[CH2:12][CH:9]([CH2:7][NH2:8])[CH2:10]2)[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1

参加物

6

反応物 4

HCID 962Water3 回HCID 14798Sodium HydroxideHCID 27792901-(Diphenylmethyl)azetidine-3-carbonitrileHCID 21226445Aluminium lithium hydride

生成物 1

HCID 100378743-Aminomethyl-1-benzhydrylazetidine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A suspension of 5.7 g (0.15 mole) of lithium aluminum hydride in 200 ml of dry tetrahydrofuran was treated portionwise with 18.6 g (75 mmole) of solid 3-cyano-1-(diphenylmethyl)azetidine. When the addition was complete, the reaction was stirred at room temperature for two hours, refluxed for four hours, and stirred at room temperature for 18 hours. The reaction was decomposed by the successive addition of 6 ml of water, 6 ml of 15% sodium hydroxide, and 18 ml of water, titrating the final water addition to give a granular precipitate. The inorganic precipitate was removed by filtration, washed with tetra hydrofuran and evaporated in vacuo to give 16.9 g of 1-(diphenylmethyl)-3-azetidinemethanamine as a heavy oil.

後処理

  1. additionWhen the addition
  2. temperaturerefluxed for four hours
  3. stirringstirred at room temperature for 18 hours
  4. customto give a granular precipitate
  5. customThe inorganic precipitate was removed by filtration
  6. washwashed with tetra hydrofuran
  7. customevaporated in vacuo

出典と根拠

ORDレコード
ord-192c2a27cfde47929379ffacfe63a01c
出典データセット
uspto-grants-1988_09
特許番号
US04771054

反応ノート

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