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

HRID 893333

反応式

HRID 893333 の反応式
[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

参加物

4

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-034a78a200814a57a5f7556d7620a45f
出典データセット
uspto-grants-1992_06
特許番号
US05124332

関連ノート

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