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1-Propylpyrrolidine-2,4-dione → HCID 19895507、化合物

HRID 892470
ノート
印刷プレビュー

反応式

HRID 892470 の反応式
C([CH:6]1[C:10](=O)[CH2:9][N:8]([CH2:12][CH2:13][CH3:14])[C:7]1=[O:15])(OCC)=O.C(N1CC(=O)CC1=O)CC.[NH2:26][C:27]1[C:31]([C:32]([O:34][CH3:35])=[O:33])=[CH:30][S:29][C:28]=1[CH2:36][CH2:37][CH2:38][CH2:39][CH3:40].O.C1(C)C=CC=CC=1>C(#N)C.C1(C)C=CC=CC=1>[CH2:12]([N:8]1[CH2:9][C:10]([NH:26][C:27]2[C:31]([C:32]([O:34][CH3:35])=[O:33])=[CH:30][S:29][C:28]=2[CH2:36][CH2:37][CH2:38][CH2:39][CH3:40])=[CH:6][C:7]1=[O:15])[CH2:13][CH3:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 135603831-Propylpyrrolidine-2,4-dioneHCID 14074904HCID 14074904、化合物HCID 19895520HCID 19895520、化合物HCID 22272177Toluene water

生成物 1

HCID 19895507HCID 19895507、化合物収率 94.2%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒
HCID 6342
Acetonitrile
溶媒

実験手順

Freshly prepared 1-propyl-Z,4-dioxopyrrolidine was prepared as described in Example le from 3-carboethoxy-1-propyl-2,4-dioxopyrrolidine (3.55 g) in acetonitrile (100 ml). The 1-propyl-2,4-dioxopyrrolidine was mixed with methyl 3-amino-2-pentylthiophene- 4-carboxylate (2.70 g) in toluene (65 ml). The mixture was refluxed for 2 hours with removal of the water/toluene azeotrope using a Dean-Stark trap. After distilling off the excess toluene, the residue was taken up in ethyl acetate, washed sequentially with saturated aqueous Na2CO3 and brine, then dried (Na2SO4) and concentrated. Chromatographic purification over silica gel afforded the title product (3.92 g, 94%) as a yellow oil; tlc, Rf =0.12, silica gel, ethyl acetate:hexane (1:1). c. 5,6-Dihydro-8-hydroxy-3-pentyl-6-propyl-pyrrolo[3,4-b]thieno[3,4-e]pyridin-7(1H)-one (Formula VII, n=1, X=N, Ra=pentyl, Rb=propyl, W=OH)

後処理

  1. distillationAfter distilling off the excess toluene
  2. washwashed sequentially with saturated aqueous Na2CO3 and brine
  3. dry with materialdried (Na2SO4)
  4. concentrationconcentrated
  5. customChromatographic purification over silica gel

出典と根拠

ORDレコード
ord-14961baf361140eca24ef16cc45b3fd7
出典データセット
uspto-grants-1992_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05118688

反応ノート

読み込み中…

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