Dimethylformamide → HCID 178496340、化合物

HRID 127683

反応式

HRID 127683 の反応式
[NH2:1][C:2]1[N+:7]([O-:8])=[C:6]([NH2:9])[CH:5]=[C:4]([Cl:10])[N:3]=1.CN(C)C=O.[CH3:16][O:17][CH2:18][CH2:19][O:20][C:21](Cl)=[O:22]>C(N(CC)CC)C>[NH2:1][C:2]1[N+:7]([O-:8])=[C:6]([NH:9][C:21]([O:20][CH2:19][CH2:18][O:17][CH3:16])=[O:22])[CH:5]=[C:4]([Cl:10])[N:3]=1

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 694002-Methoxyethyl chloroformateHCID 178507684HCID 178507684、化合物

生成物 1

HCID 178496340HCID 178496340、化合物

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

5 G. of 2,4-diamino-6-chloropyrimidine-3-oxide are suspended in 50 ml. of dimethylformamide and 5 ml. of triethylamine and cooled to 0° C. while stirring. 4.3 G. of chloroformic acid 2-methoxyethyl ester are added dropwise to the cold suspension in the course of 15 minutes. The mixture is cooled for 2 hours and then stirred at room temperature for 16 hours. The solvent is distilled off at 25° C. in a high vacuum and the residue is digested with methylene chloride. The precipitate obtained is filtered off and washed with methylene chloride, methanol and water. The filtrate is washed with water and dried over sodium sulfate. By concentrating the solvent, there is obtained pure 2-methoxyethyl 2-amino-6-chloro-4-pyrimidinecarbamate-3-oxide having a melting point of 176°-178° C. Additional material is obtained by subjecting the mother liquor to chromatographical separation on silica gel.

後処理

  1. temperatureThe mixture is cooled for 2 hours
  2. stirringstirred at room temperature for 16 hours
  3. distillationThe solvent is distilled off at 25° C. in a high vacuum
  4. customThe precipitate obtained
  5. filtrationis filtered off
  6. washwashed with methylene chloride, methanol and water
  7. washThe filtrate is washed with water
  8. dry with materialdried over sodium sulfate
  9. concentrationBy concentrating the solvent

出典と根拠

ORDレコード
ord-1a321ca1ba284e5c9a05ac59db3a1ea5
出典データセット
uspto-grants-1981_03
特許番号
US04256886

関連ノート

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