Hydrochloric Acid → HCID 67095239、化合物

HRID 2112077ノート

反応式

HRID 2112077 の反応式
[N+:1]([C:4]1[CH:12]=[CH:11][CH:10]=[C:9]2[C:5]=1[C:6](=[O:13])[NH:7][NH:8]2)([O-:3])=[O:2].[CH3:14]I.Cl>CN(C)C(=O)C>[CH3:14][N:8]1[C:9]2[C:5](=[C:4]([N+:1]([O-:3])=[O:2])[CH:12]=[CH:11][CH:10]=2)[C:6](=[O:13])[NH:7]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 6328Methyl iodideHCID 247281924-Nitro-1,2-dihydro-3H-indazol-3-one

生成物 1

HCID 67095239HCID 67095239、化合物

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

306 mg (1.7 mmol) 4-nitro-1,2-dihydro-indazol-3-one are dissolved in 1 ml N,N-dimethyl-acetamide, combined with 150 μl (2.4 mmol) methyl iodide and 500 μl (2.32 mmol) of N-ethyldiisopropylamide and stirred for 2 h at ambient temperature. Then the reaction mixture is combined with 40 ml of a 1 N aqueous hydrochloric acid and extracted twice with 50 ml dichloromethane. Then the organic phase is dried with MgSO4, the solvent is eliminated in vacuo and the crude product is purified by chromatography. The carrier used is C18-RP-silica gel and a gradient is run through which consists of 95% water and 5% acetonitrile at the starting point and 5% water and 95% acetonitrile at the finishing point.

後処理

  1. extractionextracted twice with 50 ml dichloromethane
  2. dry with materialThen the organic phase is dried with MgSO4
  3. customthe crude product is purified by chromatography

出典と根拠

ORDレコード
ord-08a147b6f56d478990c0f87e92ca21e1
出典データセット
uspto-grants-2009_04
特許番号
US07521457B2

反応ノート

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