Triethylamine → Methyl 4-[(2,5-dioxopyrrolidin-1-yl)oxy]-4-oxobutanoate

HRID 624548ノート

反応式

HRID 624548 の反応式
[OH:1][N:2]1[C:6](=[O:7])[CH2:5][CH2:4][C:3]1=[O:8].[CH3:9][O:10][C:11](=[O:17])[CH2:12][CH2:13][C:14](Cl)=[O:15].C(N(CC)CC)C>C(OCC)(=O)C>[CH3:9][O:10][C:11](=[O:17])[CH2:12][CH2:13][C:14]([O:1][N:2]1[C:6](=[O:7])[CH2:5][CH2:4][C:3]1=[O:8])=[O:15]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 73888Butanoic acid, 4-chloro-4-oxo-, methyl esterHCID 80170N-Hydroxysuccinimide

生成物 1

HCID 13798889Methyl 4-[(2,5-dioxopyrrolidin-1-yl)oxy]-4-oxobutanoate

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 1-hydroxy-pyrrolidine-2,5-dione (1.23 mL, 10 mmol) in ethyl acetate (50 mL) was added 3-chlorocarbonyl-propionic acid methyl ester (1.15 g, 10 mmol). The mixture was cooled in an ice bath. Triethylamine (1.4 mL, 10 mmol) was added dropwise. The resulting suspension was stirred for 10 min in an ice bath and for 5 min without ice bath. The white solid was removed by filtration and washed with ethyl acetate (3×3 mL). The filtrate was concentrated to a white solid (2.32 g).

後処理

  1. temperatureThe mixture was cooled in an ice bath
  2. customThe white solid was removed by filtration
  3. washwashed with ethyl acetate (3×3 mL)
  4. concentrationThe filtrate was concentrated to a white solid (2.32 g)

出典と根拠

ORDレコード
ord-fa6b295db93f4431a384e23a204b532d
出典データセット
uspto-grants-2016_04
特許番号
US09303041B2

反応ノート

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