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Aluminium lithium hydride → HCID 67983173, 화합물

HRID 530880
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HRID 530880 반응식
[F:1][C:2]1[CH:25]=[CH:24][CH:23]=[CH:22][C:3]=1[CH2:4][C:5]1([C:18](OC)=[O:19])[CH2:10][CH2:9][CH2:8][N:7]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:6]1.[H-].[Al+3].[Li+].[H-].[H-].[H-]>O1CCCC1>[F:1][C:2]1[CH:25]=[CH:24][CH:23]=[CH:22][C:3]=1[CH2:4][C:5]1([CH2:18][OH:19])[CH2:10][CH2:9][CH2:8][N:7]([C:11]([O:13][C:14]([CH3:17])([CH3:15])[CH3:16])=[O:12])[CH2:6]1
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참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 679853881-tert-Butyl 3-methyl 3-(2-fluorobenzyl)piperidine-1,3-dicarboxylate

생성물 1

HCID 67983173HCID 67983173, 화합물수율 99.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

In a flask, 1-tert-butyl 3-methyl 3-(2-fluorobenzyl)piperidine-1,3-dicarboxylate (1.41 g, 4.0 mmol) was dissolved in tetrahydrofuran (20 mL). Lithium aluminum hydride (8.03 mmol) was added to the flask. The reaction was stirred for an hour at room temperature. Upon completion, the reaction was quenched with ethyl acetate (10 ml) drop-wise. Water (30 mL) was added to the reaction. The reaction mixture then was extracted 3 times with ethyl acetate (50 mL). The organic layers were combined, were dried with sodium sulfate, concentrated and purified using flash chromatography (0 60% ethyl acetate in hexane) to give the titled compound (1.29 g).

후처리

  1. customUpon completion, the reaction was quenched with ethyl acetate (10 ml) drop-wise
  2. additionWater (30 mL) was added to the reaction
  3. extractionThe reaction mixture then was extracted 3 times with ethyl acetate (50 mL)
  4. dry with materialwere dried with sodium sulfate
  5. concentrationconcentrated
  6. custompurified

출처 및 근거

ORD 기록
ord-576b86b8857e4aab8e42bee19e5bccea
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09351965B2

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