Oxalyl chloride → 4-(N,N-diethylaminomethyl)benzoyl chloride hydrochloride

HRID 1731728ノート

反応式

HRID 1731728 の反応式
[ClH:1].[CH2:2]([N:4]([CH2:7][C:8]1[CH:16]=[CH:15][C:11]([C:12](O)=[O:13])=[CH:10][CH:9]=1)[CH2:5][CH3:6])[CH3:3].C(Cl)(=O)C([Cl:20])=O>C(Cl)Cl>[ClH:20].[CH2:2]([N:4]([CH2:7][C:8]1[CH:9]=[CH:10][C:11]([C:12]([Cl:1])=[O:13])=[CH:15][CH:16]=1)[CH2:5][CH3:6])[CH3:3]

参加物

4

反応物 2

HCID 65578Oxalyl chlorideHCID 122990074-((Diethylamino)methyl)benzoic acid hydrochloride

生成物 1

HCID 867411094-(N,N-diethylaminomethyl)benzoyl chloride hydrochloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a well-stirred suspension consisting of 1.34 g. (5.0 mmole) of 4-(N,N-diethylaminomethyl)benzoic acid hydrochloride (the product of Preparation G) in 25 ml. of methylene chloride under a nitrogen atmosphere, there was added over a five-minute period a solution consisting of 1.5 g. (0.0118 mole) of oxalyl chloride dissolved in 5 ml. of methylene chloride. The resulting reaction mixture was refluxed for a period of 17 hours and then cooled to room temperature (~20° C.). The colorless solution so obtained was evaporated under reduced pressure, and the resulting residue was washed twice with methylene chloride and then stripped free of solvent to give a white solid product. In this way, there was readily obtained substantially pure 4-(N,N-diethylaminomethyl)benzoyl chloride hydrochloride, which was used in the next reaction step without any further purification being necessary. The yield of product was assumed to be quantitative.

後処理

  1. customThe resulting reaction mixture
  2. temperaturewas refluxed for a period of 17 hours
  3. customThe colorless solution so obtained
  4. customwas evaporated under reduced pressure
  5. washthe resulting residue was washed twice with methylene chloride
  6. customto give a white solid product

出典と根拠

ORDレコード
ord-56123fedfe2048a2b710b8e347bbfc82
出典データセット
uspto-grants-1986_11
特許番号
US04623486

反応ノート

読み込み中…