Water → N-[1-(3-Dimethylaminopropyl)piperidin-4-yl]-N-methylamine

HRID 492911노트

반응식

HRID 492911 반응식
[CH3:1][N:2]([CH3:21])[CH2:3][CH2:4][C:5]([N:7]1[CH2:12][CH2:11][CH:10]([NH:13][C:14](=O)OC(C)(C)C)[CH2:9][CH2:8]1)=O.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[CH3:21][N:2]([CH3:1])[CH2:3][CH2:4][CH2:5][N:7]1[CH2:8][CH2:9][CH:10]([NH:13][CH3:14])[CH2:11][CH2:12]1

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 57677405Tert-butyl[1-(3-dimethylaminopropionyl)piperidin-4-yl]carbamate

생성물 1

HCID 23153255N-[1-(3-Dimethylaminopropyl)piperidin-4-yl]-N-methylamine수율 83.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of tert-butyl [1-(3-dimethylaminopropionyl)piperidin-4-yl]carbamate (2.73 g) in tetrahydrofuran (30 ml) was stirred in an ice bath, and lithium aluminum hydride (1.04 g) was gradually added thereto. The mixture was stirred under a nitrogen atmosphere, for 15 minutes in an ice bath and for 15 minutes at room temperature. It was further heated to reflux for 7 hours under a nitrogen atmosphere. The reaction mixture was cooled in an ice bath, and then water (1.0 ml), 5N aqueous sodium hydroxide (1.0 ml) and water (5.0 ml) were added thereto in that order and stirring was carried out on ice. The insoluble portion was filtered. The filtrate was concentrated to provide the title compound (1.51 g, 83.2%) as a pale yellow oil.

후처리

  1. temperatureIt was further heated
  2. temperatureto reflux for 7 hours under a nitrogen atmosphere
  3. temperatureThe reaction mixture was cooled in an ice bath
  4. stirringin that order and stirring
  5. filtrationThe insoluble portion was filtered
  6. concentrationThe filtrate was concentrated

출처 및 근거

ORD 기록
ord-71ddb3b7d94949dfad61232b0f225c7d
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07531532B2

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