Phthalic Acid → tert-Butyl 1-oxa-6-azaspiro(2.5)octane-6-carboxylate

HRID 47310

반응식

HRID 47310 반응식
[CH2:1]=[C:2]1[CH2:7][CH2:6][N:5]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH2:4][CH2:3]1.C(O)(=O)C1C(=CC=CC=1)C(O)=[O:19].C(=O)(O)[O-].[Na+]>CO>[O:19]1[C:2]2([CH2:7][CH2:6][N:5]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH2:4][CH2:3]2)[CH2:1]1

참가 물질

5

반응물 3

HCID 1017Phthalic AcidHCID 516892Sodium BicarbonateHCID 27568081-Boc-4-Methylenepiperidine

생성물 1

HCID 22135564tert-Butyl 1-oxa-6-azaspiro(2.5)octane-6-carboxylate수율 83.6%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

13.5 g of tert-butyl 4-methylene-1-piperidinecarboxylate was dissolved in 300 ml methanol, and 28.3 g phthalic acid monoperacid magnesium salt and 8.62 g sodium bicarbonate were added thereto, and the mixture was stirred at room temperature for 1 day. The reaction solution was filtered through Celite, and the resulting filtrate was evaporated. Ethyl acetate was added to the resulting residue which was then washed with water and brine, dried over anhydrous magnesium sulfate, and then filtered. The filtrate was evaporated, and subjected to silica gel column chromatography to give 12.2 g of tert-butyl 1-oxa-6-azaspiro[2.5]octane-6-carboxylate.

후처리

  1. filtrationThe reaction solution was filtered through Celite
  2. customthe resulting filtrate was evaporated
  3. additionEthyl acetate was added to the resulting residue which
  4. washwas then washed with water and brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. customThe filtrate was evaporated

출처 및 근거

ORD 기록
ord-88932765c1a24248bf34df8e7ab3a97d
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06699870B2

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