Water → Phthalylglycine aldehyde

HRID 606122

反応式

HRID 606122 の反応式
O.FC(F)(F)C(O)=O.C([O:11][CH:12](OCC)[CH2:13][N:14]1[C:18](=[O:19])[C:17]2=[CH:20][CH:21]=[CH:22][CH:23]=[C:16]2[C:15]1=[O:24])C>C(Cl)(Cl)Cl>[O:24]=[C:15]1[C:16]2[C:17](=[CH:20][CH:21]=[CH:22][CH:23]=2)[C:18](=[O:19])[N:14]1[CH2:13][CH:12]=[O:11]

参加物

5

反応物 3

HCID 962WaterHCID 6422Trifluoroacetic acidHCID 3152862-Phthalimidoacetaldehyde Diethyl Acetal

生成物 1

HCID 76201Phthalylglycine aldehyde収率 65.8%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

Water (50 mL) and trifluoroacetic acid (50 mL) were added to a solution of phthalimidoacetaldehyde diethyl acetal (30.0 g, 114 mmol) in chloroform (200 mL), and the reaction mixture was stirred at room temperature for 48 hours. The aqueous layer was separated, adjusted to pH 7 with the addition of sodium carbonate, and extracted with several portions of dichloromethane. The combined organic fractions were dried over magnesium sulfate, filtered, and concentrated under reduced pressure to provide 14.2 g of (1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)acetaldehyde as a white solid.

後処理

  1. customThe aqueous layer was separated
  2. additionadjusted to pH 7 with the addition of sodium carbonate
  3. extractionextracted with several portions of dichloromethane
  4. dry with materialThe combined organic fractions were dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-7ef28f501bb744008f701a1198c8f3c7
出典データセット
uspto-grants-2011_03
特許番号
US07915281B2

関連ノート

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