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Lithium aluminum hydride → HCID 58365113, 화합물

HRID 60296
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HRID 60296 반응식
[CH2:1]([C:3]1([C:16](OC(C)(C)C)=[O:17])[CH2:8][CH2:7][N:6]([C:9](OC(C)(C)C)=O)[CH2:5][CH2:4]1)[CH3:2].[AlH4-].[Li+]>O1CCCC1.[OH-].[Na+]>[CH2:1]([C:3]1([CH2:16][OH:17])[CH2:8][CH2:7][N:6]([CH3:9])[CH2:5][CH2:4]1)[CH3:2]
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참가 물질

5

반응물 2

HCID 28112Lithium aluminum hydrideHCID 67298746Di-tert-butyl 4-ethylpiperidine-1,4-dicarboxylate

생성물 1

HCID 58365113HCID 58365113, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 14798Sodium Hydroxide용매

실험 절차

To a stirred suspension of di-tert-butyl 4-ethylpiperidine-1,4-dicarboxylate (1.1 g, 3.7 mmol) in tetrahydrofuran (13 mL) was added lithium tetrahydroaluminate (1.0N solution in tetrahydrofuran, 15 mL, 15 mmol), and the mixture was stirred at ambient temperature for 6 hours. The mixture was diluted with a 1N sodium hydroxide solution (5 mL), filtered over Whatman filter paper, and the solids were washed with ethyl acetate (50 mL). The combined filtrate was separated, and the organic portion was dried over sodium sulfate, filtered, and concentrated in vacuo to afford the title compound as a white solid, which was used in the next step without any further purification (506 mg, 57%).

후처리

  1. filtrationfiltered over Whatman
  2. filtrationfilter paper
  3. washthe solids were washed with ethyl acetate (50 mL)
  4. customThe combined filtrate was separated
  5. dry with materialthe organic portion was dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-942c7aa5ec8b443fa9511366a4107558
출처 데이터셋
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09440976B2

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