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

HRID 47308

反応式

HRID 47308 の反応式
[CH2:1]=[C:2]1[CH2:7][CH2:6][N:5]([C:8]([O:10][CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[O:9])[CH2:4][CH2:3]1.C(O)(=O)C1C(=CC=CC=1)C(O)=[O:22].C(=O)(O)[O-].[Na+]>CO>[O:22]1[C:2]2([CH2:7][CH2:6][N:5]([C:8]([O:10][CH2:11][C:12]3[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=3)=[O:9])[CH2:4][CH2:3]2)[CH2:1]1

参加物

5

反応物 3

HCID 1017Phthalic AcidHCID 516892Sodium BicarbonateHCID 15519136Benzyl 4-methylidenepiperidine-1-carboxylate

生成物 1

HCID 13016598Benzyl 1-oxa-6-azaspiro(2.5)octane-6-carboxylate収率 71.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

14.7 g of benzyl 4-methylene-1-piperidinecarboxylate was dissolved in 300 ml methanol, 20.4 g of phthalic acid monoperacid magnesium salt and 13.3 g of sodium bicarbonate were added thereto, and the mixture was stirred at room temperature for 7.5 hr. The reaction solution 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 then subjected to silica gel column chromatography to give 11.3 g of benzyl 1-oxa-6-azaspiro[2.5]octane-6-carboxylate.

後処理

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

出典と根拠

ORDレコード
ord-9e9da809d2ca4d10a326e91be1998ec9
出典データセット
uspto-grants-2004_03
特許番号
US06699870B2

関連ノート

読み込み中…