Formaldehyde → Ranisen

HRID 65762

반응식

HRID 65762 반응식
[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]

참가 물질

8

반응물 3

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

생성물 1

HCID 5039Ranisen

시약·촉매·용매 4

HCID 176Acetic Acid용매2회HCID 313Hydrochloric Acid용매HCID 962Water용매HCID 11430Potassium Carbonate용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-96c1dc2b93d34428a79bb765cbb242c8
출처 데이터셋
uspto-grants-1978_12
특허 번호
US04128658

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