Water → 3-Aminomethyl-1-benzhydrylazetidine

HRID 622550노트

반응식

HRID 622550 반응식
[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

참가 물질

6

반응물 4

HCID 962Water3회HCID 14798Sodium HydroxideHCID 27792901-(Diphenylmethyl)azetidine-3-carbonitrileHCID 21226445Aluminium lithium hydride

생성물 1

HCID 100378743-Aminomethyl-1-benzhydrylazetidine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-192c2a27cfde47929379ffacfe63a01c
출처 데이터셋
uspto-grants-1988_09
특허 번호
US04771054

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