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Aluminium lithium hydride → HCID 67983173、化合物

HRID 530880
ノート
印刷プレビュー

反応式

HRID 530880 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 67983173HCID 67983173、化合物収率 99.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-576b86b8857e4aab8e42bee19e5bccea
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09351965B2

反応ノート

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