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HCID 4715295、化合物 → HCID 54475514、化合物

HRID 1363678
ノート
印刷プレビュー

反応式

HRID 1363678 の反応式
[CH2:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH:9]=[CH:10][C:11](O)=[O:12])[CH3:2].[H-].[H-].[H-].[H-].[Li+].[Al+3]>C1COCC1.[Pd]>[CH2:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:9][CH2:10][CH2:11][OH:12])[CH3:2]
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

5

反応物 2

HCID 4715295HCID 4715295、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 54475514HCID 54475514、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

3-(2-Ethyl-phenyl)-acrylic acid (17.00 g, 96.60 mmol) in THF was mixed with Pd/C (1.50 g) and hydrogenated at 50 psi for 6 hours. The resulting mixture was filtered through a pad of celite and the filtrate was concentrated. The residue was dissolved in THF and cooled to 0° C. LAH (100.00 mL, 1.0 M in THF, 0.10 mol) was added and the reaction mixture was stirred for 14 hours. The resulting mixture was quenched with NaOH and extracted with Et2O (3×250 mL). The combined organic extracts were washed with H2O (3×150 mL) and brine (1×150 mL), then dried over MgSO4 and concentrated to give the title alcohol.

後処理

  1. filtrationThe resulting mixture was filtered through a pad of celite
  2. concentrationthe filtrate was concentrated
  3. dissolutionThe residue was dissolved in THF
  4. customThe resulting mixture was quenched with NaOH
  5. extractionextracted with Et2O (3×250 mL)
  6. washThe combined organic extracts were washed with H2O (3×150 mL) and brine (1×150 mL)
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-b485ca1236294d869daec536ffad7de2
出典データセット
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07884244B2

反応ノート

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