Oxalyl chloride → 3-(4-Nitrophenyl)propionyl chloride

HRID 356474

反応式

HRID 356474 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([CH2:10][CH2:11][C:12]([OH:14])=O)=[CH:6][CH:5]=1)([O-:3])=[O:2].C(Cl)(=O)C([Cl:18])=O>C(Cl)Cl.CN(C=O)C>[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([CH2:10][CH2:11][C:12]([Cl:18])=[O:14])=[CH:6][CH:5]=1)([O-:3])=[O:2]

参加物

5

反応物 2

HCID 65578Oxalyl chlorideHCID 855263-(4-Nitrophenyl)propanoic acid

生成物 1

HCID 147973603-(4-Nitrophenyl)propionyl chloride

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide触媒HCID 6344Dichloromethane溶媒

実験手順

3-(4-Nitrophenyl)propanoic acid prepared in Example DD (12.5 g, 64 mmol) was suspended in CH2Cl2 (300 mL) and treated with oxalyl chloride (7.4 mL, 85 mmol) and DMF (5 drops). The solution was stirred overnight at room temperature. The solution was concentrated, and the residue was dissolved in CH2Cl2 and re-concentrated. The crude product was used as is in the next step.

後処理

  1. concentrationThe solution was concentrated
  2. dissolutionthe residue was dissolved in CH2Cl2
  3. concentrationre-concentrated

出典と根拠

ORDレコード
ord-9d995b24aa6f4bc1bc16cc3926527678
出典データセット
uspto-grants-1998_11
特許番号
US05834506

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