Chloroform → HCID 86667593、化合物

HRID 85304ノート

反応式

HRID 85304 の反応式
P(Cl)(Cl)(Cl)=O.[CH2:6]([NH:10][C:11]1[CH:16]=[C:15]([O:17][CH3:18])[CH:14]=[C:13]([O:19][CH3:20])[CH:12]=1)[CH2:7][CH2:8][CH3:9].C(Cl)(Cl)Cl.CN(C)[CH:27]=[O:28]>>[CH2:6]([N:10]([CH2:6][CH2:7][CH2:8][CH3:9])[C:11]1[CH:16]=[C:15]([O:17][CH3:18])[C:14]([CH:27]=[O:28])=[C:13]([O:19][CH3:20])[CH:12]=1)[CH2:7][CH2:8][CH3:9]

参加物

5

反応物 4

HCID 6212ChloroformHCID 6228Dimethylformamide2 回HCID 24813Phosphorus oxychlorideHCID 137939884-Butylamino-2,6-dimethoxybenzene

生成物 1

HCID 86667593HCID 86667593、化合物収率 80%

反応条件

温度
7.5 °C

実験手順

In a stream of argon, to 30 ml of N,N-dimethylformamide was added 16.0 g (104 mmol) of phosphorus oxychloride under cooling at 5 to 10° C. and stirring. After the mixture was well-stirred, 23.5 g (80.1 mmol) of 4-butylamino-2,6-dimethoxybenzene dissolved in 10 ml of N,N-dimethylformamide was added dropwise. The mixture was reacted with stirring for 1.5 hours. After the mixture was poured into 70 ml of ice water, extraction with 200 ml of chloroform, washing with a saturated saline solution, drying over anhydrous magnesium sulfate, and concentration were performed. The residue was purified by silica gel chromatography to give 18.8 g (yield: 80%) of 4-dibutylamino-2,6-dimethoxybenzaldehyde as a dark purple crystal (mp: 55-56° C.)

後処理

  1. stirringAfter the mixture was well-stirred
  2. additionwas added dropwise
  3. customThe mixture was reacted
  4. stirringwith stirring for 1.5 hours
  5. washwashing with a saturated saline solution
  6. dry with materialdrying over anhydrous magnesium sulfate, and concentration
  7. customThe residue was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-46197a9033de47c596ab244156fbcaf9
出典データセット
uspto-grants-2014_09
特許番号
US08846955B2

反応ノート

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