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

HRID 624548노트

반응식

HRID 624548 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-fa6b295db93f4431a384e23a204b532d
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09303041B2

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