Dabco → N,N-dimethyl-3-methoxyimino-2-[(methylcarbamoyl)oximino]butyramide

HRID 26711

反応式

HRID 26711 の反応式
[CH3:1][N:2]([CH3:13])[C:3](=[O:12])[C:4](=[N:10][OH:11])[C:5](=[N:7][O:8][CH3:9])[CH3:6].[CH3:14][N:15]=[C:16]=[O:17].C1N2CCN(CC2)C1>C(Cl)Cl>[CH3:13][N:2]([CH3:1])[C:3](=[O:12])[C:4](=[N:10][O:11][C:16](=[O:17])[NH:15][CH3:14])[C:5](=[N:7][O:8][CH3:9])[CH3:6]

参加物

5

反応条件

温度
25 °C

実験手順

A mixture of 34 parts of N,N-dimethyl-2-hydroxyimino-3-methoxyiminobutyramide, 350 parts of methylene chloride, 13 parts of methyl isocyanate and one-tenth part triethylenediamine was stirred at 25° C. for 3 hours and then refluxed for 1 hour. The solvent was removed by stripping under reduced pressure (15 mm.) at 50° bath temperature, thereby affording the solid crude product. Recrystallization from a benzene-acetonitrile mixture gave 32 parts of N,N-dimethyl-3-methoxyimino-2-[(methylcarbamoyl)oximino]butyramide, m.p. 172°-173° C.

後処理

  1. temperaturerefluxed for 1 hour
  2. customThe solvent was removed
  3. customby stripping under reduced pressure (15 mm.) at 50°
  4. customaffording the solid crude product
  5. customRecrystallization from a benzene-acetonitrile mixture

出典と根拠

ORDレコード
ord-515cd4a944c94100a0ce420c1a056260
出典データセット
uspto-grants-1979_04
特許番号
US04151296

関連ノート

読み込み中…