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

HRID 40985

반응식

HRID 40985 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

반응 조건

온도
0 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-5c426494f53b403092b47b43b4284363
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08530485B2

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