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Ammonium Chloride → Ethyl 4-ethyl-6-[methyl(2-thienylsulfonyl)amino]-1,4-dihydropyrrolo[3,2-b]pyrrole-2-carboxylate

HRID 453596
ノート
印刷プレビュー

反応式

HRID 453596 の反応式
[O-]CC.[Na+].[CH2:5]([N:7]1[C:11]([CH:12]=O)=[CH:10][C:9]([N:14]([CH3:23])[S:15]([C:18]2[S:19][CH:20]=[CH:21][CH:22]=2)(=[O:17])=[O:16])=[CH:8]1)[CH3:6].[N:24]([CH2:27][C:28]([O:30][CH2:31][CH3:32])=[O:29])=[N+]=[N-].[Cl-].[NH4+]>C(O)C>[CH2:5]([N:7]1[C:11]2[CH:12]=[C:27]([C:28]([O:30][CH2:31][CH3:32])=[O:29])[NH:24][C:10]=2[C:9]([N:14]([CH3:23])[S:15]([C:18]2[S:19][CH:20]=[CH:21][CH:22]=2)(=[O:17])=[O:16])=[CH:8]1)[CH3:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 25517Ammonium ChlorideHCID 69480Acetic acid, azido-, ethyl esterHCID 2723922Sodium ethoxideHCID 59411382N-(1-ethyl-5-formyl-1H-pyrrol-3-yl)-N-methylthiophene-2-sulfonamide

生成物 1

HCID 59411371Ethyl 4-ethyl-6-[methyl(2-thienylsulfonyl)amino]-1,4-dihydropyrrolo[3,2-b]pyrrole-2-carboxylate収率 32%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution (150 mL) of sodium ethoxide (8.3 g) in ethanol was added dropwise a mixture of N-(1-ethyl-5-formyl-1H-pyrrol-3-yl)-N-methylthiophene-2-sulfonamide (8.5 g) and ethyl azidoacetate (16.5 g) under ice-cooling. After the completion of the dropwise addition, the mixture was stirred for 2 hr. Saturated aqueous ammonium chloride solution was added to the reaction mixture, and the mixture was concentrated. The obtained residue was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated brine, dried (MgSO4) and concentrated. The obtained residue was subjected to silica gel column chromatography and eluted with ethyl acetate-hexane (1:1, volume ratio). The obtained yellow oil was dissolved in toluene (50 mL), and the mixture was stirred at 110° C. for 1 hr. The reaction mixture was concentrated, and the residue was subjected to silica gel column chromatography to give ethyl 4-ethyl-6-[methyl(2-thienylsulfonyl)amino]-1,4-dihydropyrrolo[3,2-b]pyrrole-2-carboxylate (1.12 g, yield 32%) as colorless crystals from a fraction eluted with ethyl acetate-hexane (1:1, volume ratio). melting point 122° C.

後処理

  1. temperaturecooling
  2. additionAfter the completion of the dropwise addition
  3. concentrationthe mixture was concentrated
  4. extractionThe obtained residue was extracted with ethyl acetate
  5. washThe ethyl acetate layer was washed with saturated brine
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated
  8. washeluted with ethyl acetate-hexane (1:1, volume ratio)
  9. dissolutionThe obtained yellow oil was dissolved in toluene (50 mL)
  10. stirringthe mixture was stirred at 110° C. for 1 hr
  11. concentrationThe reaction mixture was concentrated

出典と根拠

ORDレコード
ord-f0f1584f1b2d49ca9b8b4bd71be46f62
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08492405B2

反応ノート

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