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

HRID 36668

反応式

HRID 36668 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-f0e21d3541234709a7e0200795083ab8
出典データセット
uspto-grants-1995_05
特許番号
US05416096

関連ノート

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