Benzylamine → 1-[(Benzylcarbamoyl)oxy]pyrrolidine-2,5-dione

HRID 744899ノート

反応式

HRID 744899 の反応式
C1C(=O)N(O[C:9]([O:11][N:12]2[C:17](=[O:18])[CH2:16][CH2:15][C:13]2=[O:14])=[O:10])C(=O)C1.[CH2:19]([NH2:26])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>C(#N)C>[CH2:19]([NH:26][C:9](=[O:10])[O:11][N:12]1[C:13](=[O:14])[CH2:15][CH2:16][C:17]1=[O:18])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1

参加物

4

反応物 2

HCID 7504BenzylamineHCID 676246Di(succinimido) carbonate

生成物 1

HCID 131119021-[(Benzylcarbamoyl)oxy]pyrrolidine-2,5-dione収率 76.2%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

18.4 g of N,N'-disuccinimidyl carbonate are added in small portions at 5° C. within 5 minutes to a solution of 6.4 g of benzylamine in 150 ml of acetonitrile. The reaction mixture is stirred at room temperature and then evaporated. The residue is taken up in ethyl acetate and washed with water. The organic phase is dried, concentrated and the residue is recrystallized from methylene chlorideohexane. 11.3 g of colourless 2,5-dioxo-pyrrolidin-1-yl benzylcarbamate, MS (FAB): 133 (M- HO-Succ), are isolated.

後処理

  1. customevaporated
  2. washwashed with water
  3. customThe organic phase is dried
  4. concentrationconcentrated
  5. customthe residue is recrystallized from methylene chlorideohexane

出典と根拠

ORDレコード
ord-b9bf4828c6d94554ac084721824d2361
出典データセット
uspto-grants-1996_09
特許番号
US05559232

反応ノート

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