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Aluminium lithium hydride → HCID 69907451、化合物

HRID 1582686
ノート
印刷プレビュー

反応式

HRID 1582686 の反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].[CH:7]1([C:15]2[CH:20]=[CH:19][C:18]([C:21]([CH3:28])=[CH:22][C:23](OCC)=[O:24])=[CH:17][CH:16]=2)[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1>CCOCC>[CH:7]1([C:15]2[CH:16]=[CH:17][C:18]([C:21]([CH3:28])=[CH:22][CH2:23][OH:24])=[CH:19][CH:20]=2)[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14]1
参加物反応条件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 69906260HCID 69906260、化合物

生成物 1

HCID 69907451HCID 69907451、化合物収率 79.3%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

反応条件

温度
0 °C

実験手順

To an ice cooled slurry of LiAlH4 (2.9 g) in dry ether (200 ml) was added a solution of ethyl 3-(4′-cyclooctylphenyl)-but-2-enoate (3d, 10 g) in dry ether (50 ml) dropwise. The reaction mixture was stirred at 0° C. for 2 h. The reaction mixture was quenched with water (11 ml). A solution of 10% NaOH (10 ml) was added and ether layer was decanted. The precipitate was washed with ether and combined extracts were concentrated. The crude product was purified by column chromatography on silica gel to give 6.82 g (79.3% yield) of 3-(4′-cyclooctylphenyl)-2-butenol (4d, formula 4, R=cyclooctyl) m.p. 40-44° C.

後処理

  1. customThe reaction mixture was quenched with water (11 ml)
  2. additionA solution of 10% NaOH (10 ml) was added
  3. customether layer was decanted
  4. washThe precipitate was washed with ether
  5. concentrationwere concentrated
  6. customThe crude product was purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-6a1a94bf357b45feb67fde86076f2be9
出典データセット
uspto-grants-2004_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06737438B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート