Hydrochloric Acid → HCID 53684414、化合物

HRID 1447200ノート

反応式

HRID 1447200 の反応式
CCN(C1C=CC=CC=1)CC.Cl[C:13]([O:15][CH3:16])=[O:14].[CH3:17][C:18]([CH3:25])=[CH:19][CH:20]=[N:21][CH:22]([CH3:24])[CH3:23].Cl>C1(C)C=CC=CC=1.O>[CH3:16][O:15][C:13](=[O:14])[N:21]([CH:22]([CH3:24])[CH3:23])[CH:20]=[CH:19][C:18]([CH3:25])=[CH2:17]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 6586Methyl chloroformateHCID 7061N,N-DiethylanilineHCID 13061751HCID 13061751、化合物

生成物 1

HCID 53684414HCID 53684414、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1140Toluene溶媒2 回

実験手順

To a stirred solution of 657 g diethylaniline in 2 liter toluene is added dropwise over ca. 5 minutes 416 g methyl chloroformate. Then to the stirred mixture 500 g N-(3-methyl-2-butenyliden)-isopropylamine in 500 ml toluene is added dropwise over 2 hours, maintaining the temperature between 25° and 30° C. Stirring is continued for 1 hour upon completion of the addition and the reaction mixture is treated with 400 ml of water and 90 ml conc. hydrochloric acid. The organic phase is washed with 600 ml of saturated aqueous sodium bicarbonate solution and with 600 ml water, dried and evaporated in vacuo to give the heading compound.

後処理

  1. temperaturemaintaining the temperature between 25° and 30° C
  2. additionis continued for 1 hour upon completion of the addition
  3. washThe organic phase is washed with 600 ml of saturated aqueous sodium bicarbonate solution and with 600 ml water
  4. customdried
  5. customevaporated in vacuo
  6. customto give the heading compound

出典と根拠

ORDレコード
ord-efc4a1e9a62b42598dca9797fa9dc3c5
出典データセット
uspto-grants-1982_02
特許番号
US04316042

反応ノート

読み込み中…