Ethyl 2-(1,4-dioxaspiro[4.5]decan-8-yl)acetate → 2-(1,4-Dioxaspiro(4.5)decan-8-yl)acetic acid

HRID 893333

반응식

HRID 893333 반응식
[O:1]1[C:5]2([CH2:10][CH2:9][CH:8]([CH2:11][C:12]([O:14]CC)=[O:13])[CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1>[OH-].[Na+].C(O)C>[O:1]1[C:5]2([CH2:10][CH2:9][CH:8]([CH2:11][C:12]([OH:14])=[O:13])[CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1

참가 물질

4

반응물 1

HCID 15700391Ethyl 2-(1,4-dioxaspiro[4.5]decan-8-yl)acetate

생성물 1

HCID 151011212-(1,4-Dioxaspiro(4.5)decan-8-yl)acetic acid수율 87.2%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 14798Sodium Hydroxide용매

실험 절차

A solution of ethyl 1,4-dioxaspiro[4,5]decane-8-acetate (50.0 g) in 50 mL of 4.8N sodium hydroxide solution and 400 mL of ethanol is refluxed under nitrogen for 2 hours. The mixture is concentrated in vacuo to remove the ethanol. The residue is acidified with a saturated sodium biphosphate solution and the mixture is extracted with ethyl acetate (2×300 mL). The organic extract is dried over magnesium sulfate, and evaporated in vacuo to give an oily solid which is triturated with hexane and filtered to give 38.25 g of the title compound as a white solid; mp 110°-113° C.

후처리

  1. concentrationThe mixture is concentrated in vacuo
  2. customto remove the ethanol
  3. extractionthe mixture is extracted with ethyl acetate (2×300 mL)
  4. extractionThe organic extract
  5. dry with materialis dried over magnesium sulfate
  6. customevaporated in vacuo
  7. customto give an oily solid which
  8. customis triturated with hexane
  9. filtrationfiltered

출처 및 근거

ORD 기록
ord-034a78a200814a57a5f7556d7620a45f
출처 데이터셋
uspto-grants-1992_06
특허 번호
US05124332

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