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Citric Acid → 4-((Tert-butoxy)carbonyl)morpholine-2-carboxylic acid

HRID 602132
ノート
印刷プレビュー

反応式

HRID 602132 の反応式
[OH-].[K+].[C:3]([O:7][C:8]([N:10]1[CH2:15][CH2:14][O:13][CH:12]([C:16]([O:18]C)=[O:17])[CH2:11]1)=[O:9])([CH3:6])([CH3:5])[CH3:4].O.C(O)(=O)CC(CC(O)=O)(C(O)=O)O>CO>[C:3]([O:7][C:8]([N:10]1[CH2:15][CH2:14][O:13][CH:12]([C:16]([OH:18])=[O:17])[CH2:11]1)=[O:9])([CH3:6])([CH3:4])[CH3:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 311Citric AcidHCID 962WaterHCID 14797Potassium HydroxideHCID 588174744-tert-Butyl 2-methyl morpholine-2,4-dicarboxylate

生成物 1

HCID 27559654-((Tert-butoxy)carbonyl)morpholine-2-carboxylic acid収率 93%

試薬・触媒・溶媒 1

HCID 887Methanol
溶媒

実験手順

A 1 mol/L aqueous potassium hydroxide solution (3 mL) was added to methyl 4-(tert-butoxycarbonyl)morpholine-2-carboxylate (251 mg, 1.02 mmol) in methanol (15 mL). The mixture was stirred at room temperature for 8 hours. Subsequently, water was added to the mixture, followed by addition of a 5% aqueous citric acid solution to make the mixture acidic. The mixture was then extracted with ethyl acetate. The extract was washed with brine and was dried over magnesium sulfate. Evaporation of the solvent gave 219 mg (93%) of the desired compound as a colorless powder.

後処理

  1. extractionThe mixture was then extracted with ethyl acetate
  2. washThe extract was washed with brine
  3. dry with materialwas dried over magnesium sulfate
  4. customEvaporation of the solvent

出典と根拠

ORDレコード
ord-52c0185b802d4cea9b27386c3abe2c19
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07902367B2

反応ノート

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