Water → HCID 85969746, 화합물

HRID 1916621노트

반응식

HRID 1916621 반응식
O.O.[Sn](Cl)Cl.C([O-])(O)=O.[Na+].[CH3:11][NH:12][C:13]1[CH:18]=[CH:17][C:16]([CH2:19][N:20]2[CH2:24][CH2:23][CH2:22][CH2:21]2)=[CH:15][C:14]=1[N+:25]([O-])=O.O>CCOC(C)=O.OS([O-])(=O)=O.[K+]>[CH3:11][NH:12][C:13]1[C:14]([NH2:25])=[CH:15][C:16]([CH2:19][N:20]2[CH2:21][CH2:22][CH2:23][CH2:24]2)=[CH:17][CH:18]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 61436Stannous chloride dihydrateHCID 516892Sodium BicarbonateHCID 62177350HCID 62177350, 화합물

생성물 1

HCID 85969746HCID 85969746, 화합물

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 516920Potassium bisulfate용매

실험 절차

4.85 g (21.5 mmol) tin(II)chloride dihydrate and 4.45 g (53.0 mmol) NaHCO3 are added to a solution of 1.00 g (4.25 mmol) methyl-(2-nitro-4-pyrrolidin-1-ylmethyl-phenyl)-amine in 60 mL EtOAc at RT. The reaction is refluxed for 2 h and then diluted with 100 mL 1 M KHSO4 solution and some water. The mixture is filtered. The aqueous phase is combined with K2CO3 and extracted twice with 80 mL EtOAc. The organic phase is dried over MgSO4 and the solvent is eliminated i.vac.

후처리

  1. temperatureThe reaction is refluxed for 2 h
  2. filtrationThe mixture is filtered
  3. extractionextracted twice with 80 mL EtOAc
  4. dry with materialThe organic phase is dried over MgSO4

출처 및 근거

ORD 기록
ord-bb4a24ea055c4c6193ded6bd577d44aa
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08618132B2

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