Sodium hydride → 5-Benzyl-4,6-dioxo-octahydropyrrolo[3,4-b]pyrrole

HRID 345801

반응식

HRID 345801 반응식
[H-].[Na+].[CH2:3]([N:10]1[C:14](=[O:15])[CH2:13][CH:12]([NH:16][CH2:17][CH2:18]Cl)[C:11]1=[O:20])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1>CN(C)C=O>[CH2:3]([N:10]1[C:14](=[O:15])[CH:13]2[CH:12]([NH:16][CH2:17][CH2:18]2)[C:11]1=[O:20])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

참가 물질

4

반응물 2

HCID 24758Sodium hydrideHCID 150700021-Benzyl-3-(2-chloroethylamino)pyrrolidine-2,5-dione

생성물 1

HCID 150700035-Benzyl-4,6-dioxo-octahydropyrrolo[3,4-b]pyrrole수율 56%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

17.4 g (0.58 mmol) of sodium hydride suspension are reacted with 119 g (0.45 mol) of 1-benzyl-3-(2-chloroethylamino)-pyrrolidine-2,5-dione in 550 ml of absolute dimethylformamide in accordance with the working instructions of Example Ib. After the mixture has been left to stand overnight, it is worked up under aqueous conditions. On purification by chromatography, impurities are first eluted with ethyl acetate and the product is then eluted with ethyl acetate:methanol (3:1) (RF value 0.55). 57.7 g of product (56% of theory) are isolated.

후처리

  1. waitAfter the mixture has been left
  2. customOn purification by chromatography, impurities
  3. washare first eluted with ethyl acetate
  4. washthe product is then eluted with ethyl acetate:methanol (3:1) (RF value 0.55)

출처 및 근거

ORD 기록
ord-60d58a63d1d54a73a53ed5a9d9914d6f
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05059597

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