Water → HCID 85969746、化合物

HRID 1916621ノート

反応式

HRID 1916621 の反応式
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

参加物

7

反応物 4

HCID 962WaterHCID 61436Stannous chloride dihydrateHCID 516892Sodium BicarbonateHCID 62177350HCID 62177350、化合物

生成物 1

HCID 85969746HCID 85969746、化合物

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 516920Potassium bisulfate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bb4a24ea055c4c6193ded6bd577d44aa
出典データセット
uspto-grants-2013_12
特許番号
US08618132B2

反応ノート

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