Water → HCID 178488949, 화합물

HRID 745437

반응식

HRID 745437 반응식
[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

참가 물질

5

반응물 3

HCID 962WaterHCID 8868Ethyl AcetoacetateHCID 2290744-Methoxybenzenecarboximidamide

생성물 1

HCID 178488949HCID 178488949, 화합물수율 75%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e992968ba96e4ce48b7d3fea3bb6058d
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04598149

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