Ethyl isothiocyanatoformate → 3-(2-Methoxy-2-methylpropyl)-2-thioxanthine

HRID 548782ノート

反応式

HRID 548782 の反応式
C(O[C:4]([N:6]=[C:7]=[S:8])=[O:5])C.[CH3:9][O:10][C:11]([CH3:23])([CH3:22])[CH2:12][NH:13][C:14]1[N:15]=[CH:16][NH:17][C:18]=1C(N)=O>C(Cl)Cl>[CH3:9][O:10][C:11]([CH3:23])([CH3:22])[CH2:12][N:13]1[C:14]2[N:15]=[CH:16][NH:17][C:18]=2[C:4](=[O:5])[NH:6][C:7]1=[S:8]

参加物

4

反応物 2

HCID 85320Ethyl isothiocyanatoformateHCID 671575204-[(2-methoxy-2-methylpropyl)amino]-1H-imidazole-5-carboxamide

生成物 1

HCID 236583763-(2-Methoxy-2-methylpropyl)-2-thioxanthine収率 32%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
50 °C

実験手順

Ethoxycarbonyl isothiocyanate (0.144 g, 1.1 mmol) was added to a stirred solution of 4-[(2-methoxy-2-methylpropyl)amino]-1H-imidazole-5-carboxamide (0.155 g, 0.73 mmol), which was obtained from Example 3(b), in CH2Cl2 (2.5 mL) at r.t. for 16 h. The solvent was evaporated and the residue was then dissolved in 2% aqueous sodium hydroxide (NaOH) solution (10 mL) and heated at 50° C. for 3 h. The pH was adjusted to neutral with 2 M HCl and the resulted precipitates were collected by filtration followed by prep-HPLC purification. The title compound was obtained as a white solid in 32% yield (60 mg).

後処理

  1. customThe solvent was evaporated
  2. dissolutionthe residue was then dissolved in 2% aqueous sodium hydroxide (NaOH) solution (10 mL)
  3. customthe resulted precipitates
  4. filtrationwere collected by filtration
  5. customfollowed by prep-HPLC purification

出典と根拠

ORDレコード
ord-c900137f21a04bed8761c60fe3fdd23e
出典データセット
uspto-grants-2011_05
特許番号
US07943625B2

反応ノート

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