Water → HCID 178488949、化合物

HRID 745437

反応式

HRID 745437 の反応式
[C:1](OCC)(=[O:6])[CH2:2][C:3]([CH3:5])=O.[CH3:10][O:11][C:12]1[CH:20]=[CH:19][C:15]([C:16]([NH2:18])=[NH:17])=[CH:14][CH:13]=1.O>C(Cl)(Cl)Cl>[OH:6][C:1]1[N:18]=[C:16]([C:15]2[CH:19]=[CH:20][C:12]([O:11][CH3:10])=[CH:13][CH:14]=2)[N:17]=[C:3]([CH3:5])[CH:2]=1

参加物

5

反応物 3

HCID 962WaterHCID 8868Ethyl AcetoacetateHCID 2290744-Methoxybenzenecarboximidamide

生成物 1

HCID 178488949HCID 178488949、化合物収率 75%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

Under N2, a solution of ethyl acetoacetate (7.15 g, 0.053 mol) in CHCl3 (200 ml) was added dropwise to a suspension of 4-methoxybenzamidine in CHCl3 (200 ml). After stirring at room temperature overnight, water was added to the solution. The aqueous phase was separated and extracted with CHCl3 and the organic layers were combined, dried (Na2SO4), filtered and concentrated to dryness. The residue was chromatographed on silica gel and the product was eluted with 2% CH3OH--CHCl3 to yield 8.58 g (75%) of product, m.p. 198°-199° C.

後処理

  1. customThe aqueous phase was separated
  2. extractionextracted with CHCl3
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated to dryness
  6. customThe residue was chromatographed on silica gel
  7. washthe product was eluted with 2% CH3OH

出典と根拠

ORDレコード
ord-e992968ba96e4ce48b7d3fea3bb6058d
出典データセット
uspto-grants-1986_07
特許番号
US04598149

関連ノート

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