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Lithium aluminum hydride → HCID 58365113、化合物

HRID 60296
ノート
印刷プレビュー

反応式

HRID 60296 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 1

HCID 58365113HCID 58365113、化合物

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-942c7aa5ec8b443fa9511366a4107558
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09440976B2

反応ノート

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