Water → 1-(diphenylmethyl)-N-ethyl-3-azetidinemethanamine

HRID 868119ノート

反応式

HRID 868119 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]1([CH:13]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[N:14]2[CH2:17][CH:16]([C:18]([NH:20][CH2:21][CH3:22])=O)[CH2:15]2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.O.[OH-].[Na+]>O1CCCC1>[C:7]1([CH:13]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[N:14]2[CH2:17][CH:16]([CH2:18][NH:20][CH2:21][CH3:22])[CH2:15]2)[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1

参加物

6

反応物 4

HCID 962Water3 回HCID 14798Sodium HydroxideHCID 13772850HCID 13772850、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 99938381-(diphenylmethyl)-N-ethyl-3-azetidinemethanamine収率 85.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a suspension of 3.2 g (85 mmole) of lithium aluminum hydride in 50 ml of dry tetrahydrofuran was added dropwise, a solution of 8.5 g (28.0 mmole) of 1-(diphenylmethyl)-N-ethyl-3-azetidinecarboxamide in 50 ml of dry tetrahydrofuran. After the addition was complete, the reaction was refluxed for two hours, cooled to room temperature, and decomposed by the successive addition of 3.4 ml of water, 3.4 ml of 15% aqueous sodium hydroxide and 10.2 ml of water, titrating the final water addition to give a granular precipitate. The inorganic precipitate was removed by filtration, washed with tetrahydrofuran and evaporated in vacuo to give 6.7 g of 1-(diphenylmethyl)-N-ethyl-3-azetidinemethanamine as a heavy syrup. This was used without further purification.

後処理

  1. additionwas added dropwise
  2. additionAfter the addition
  3. temperaturethe reaction was refluxed for two hours
  4. customto give a granular precipitate
  5. customThe inorganic precipitate was removed by filtration
  6. washwashed with tetrahydrofuran
  7. customevaporated in vacuo

出典と根拠

ORDレコード
ord-9480f46adfef47c880b778b4f8657e2f
出典データセット
uspto-grants-1988_10
特許番号
US04777175

反応ノート

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