Lithium aluminum hydride → 1,4-Dioxaspiro(4.5)decan-8-ol

HRID 40985

反応式

HRID 40985 の反応式
[O:1]1[C:5]2([CH2:10][CH2:9][C:8](=[O:11])[CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1.[AlH4-].[Li+]>CCOCC>[O:1]1[C:5]2([CH2:10][CH2:9][CH:8]([OH:11])[CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1

参加物

4

反応物 2

HCID 28112Lithium aluminum hydrideHCID 5674151,4-Dioxaspiro[4.5]decan-8-one

生成物 1

HCID 5673521,4-Dioxaspiro(4.5)decan-8-ol

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

1,4-Dioxa-spiro[4.5]decan-8-one (2.00 g, 0.0128 mol) was dissolved in ether (50 mL) and the mixture was cooled to 0° C. To the reaction was added 1 M lithium tetrahydroaluminate in ether (7.0 mL) and this mixture was stirred at 0° C. for 2 hours at which time TLC analysis showed no starting material present. The reaction was then quenched with water and 1 N NaOH (0.5 mL of each) and then filtered. The filtered solid was washed with ether and the combined ether filtrate was concentrated using a rotary evaporator to give the product. NMR (CDCl3): 3.94 (m, 4H), 3.81 (m, 1H), 1.79-1.92 (m, 4H), 1.54-1.70 (m, 4H).

後処理

  1. customThe reaction was then quenched with water and 1 N NaOH (0.5 mL of each) and
  2. filtrationthen filtered
  3. washThe filtered solid was washed with ether
  4. concentrationthe combined ether filtrate was concentrated
  5. customa rotary evaporator
  6. customto give the product

出典と根拠

ORDレコード
ord-5c426494f53b403092b47b43b4284363
出典データセット
uspto-grants-2013_09
特許番号
US08530485B2

関連ノート

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