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

HRID 868119노트

반응식

HRID 868119 반응식
[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

참가 물질

6

반응물 4

HCID 962Water3회HCID 14798Sodium HydroxideHCID 13772850HCID 13772850, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 99938381-(diphenylmethyl)-N-ethyl-3-azetidinemethanamine수율 85.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9480f46adfef47c880b778b4f8657e2f
출처 데이터셋
uspto-grants-1988_10
특허 번호
US04777175

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