Formaldehyde → Ranisen

HRID 65762

反応式

HRID 65762 の反応式
[CH3:1][N:2]([CH3:9])[CH2:3][C:4]1[O:5][CH:6]=[CH:7][CH:8]=1.[CH2:10]=O.[SH:12][CH2:13][CH2:14][NH:15][C:16]([NH:21][CH3:22])=[CH:17][N+:18]([O-:20])=[O:19]>C(O)(=O)C.Cl.O.C(=O)([O-])[O-].[K+].[K+]>[CH3:1][N:2]([CH2:3][C:4]1[O:5][C:6]([CH2:10][S:12][CH2:13][CH2:14][NH:15][C:16]([NH:21][CH3:22])=[CH:17][N+:18]([O-:20])=[O:19])=[CH:7][CH:8]=1)[CH3:9]

参加物

8

反応物 3

HCID 712FormaldehydeHCID 84478N,N-dimethyl-2-FuranmethanamineHCID 181798N-(2-Mercaptoethyl)-N'-methyl-2-nitro-1,1-ethenediamine

生成物 1

HCID 5039Ranisen

試薬・触媒・溶媒 4

HCID 176Acetic Acid溶媒2 回HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒HCID 11430Potassium Carbonate溶媒

実験手順

N,N-Dimethyl-2-furanmethanamine (125 mg) was dissolved in glacial acetic acid (1 ml) and paraformaldehyde (30 mg) added. A solution of N-(2-mercaptoethyl)-N'-methyl-2-nitro-1,1-ethenediamine (354 mg) in concentrated hydrochloric acid (1 ml) and glacial acetic acid (1 ml) was added dropwise and the mixture left to stand at room temperature for 5 days. The solution was diluted with water (30 ml), saturated with potassium carbonate and extracted with ethyl acetate. The combined extracts were purified by preparative layer chromatography to give the title compound as Example 15 (89 mg).

後処理

  1. waitthe mixture left
  2. extractionextracted with ethyl acetate
  3. customThe combined extracts were purified by preparative layer chromatography

出典と根拠

ORDレコード
ord-96c1dc2b93d34428a79bb765cbb242c8
出典データセット
uspto-grants-1978_12
特許番号
US04128658

関連ノート

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