3-Methylbenzoic acid → 3-Methylbenzoyl chloride

HRID 37185

反応式

HRID 37185 の反応式
[C:1]1([CH3:10])[CH:6]=[CH:5][CH:4]=[C:3]([C:7](O)=[O:8])[CH:2]=1.C(Cl)(=O)C([Cl:14])=O>C1C=CC=CC=1.CN(C=O)C>[CH3:10][C:1]1[CH:2]=[C:3]([CH:4]=[CH:5][CH:6]=1)[C:7]([Cl:14])=[O:8]

参加物

5

反応物 2

HCID 74183-Methylbenzoic acidHCID 65578Oxalyl chloride

生成物 1

HCID 743753-Methylbenzoyl chloride

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide触媒HCID 241Benzene溶媒

実験手順

Meanwhile, the 3-methylbenzoyl chloride acylating agent was prepared by suspending 3.016 g (22.0 mmol) of m-toluic acid in 100 ml benzene. To this solution was added 2.0 equiv. (3.84 ml) of oxalyl chloride, dropwise via a pressure-equalizing dropping funnel at O° C. DMF (2-3 drops) was added to the reaction mixture catalytically and the ice bath was removed. The progress of the reaction was monitored via infrared spectroscopy. The solvent was removed by rotary vacuum evaporation and the residual oil was pumped down under high vacuum overnight.

後処理

  1. customthe ice bath was removed
  2. customThe solvent was removed by rotary vacuum evaporation
  3. customwas pumped down under high vacuum overnight

出典と根拠

ORDレコード
ord-327c30f17ea74844a93444c148790f2c
出典データセット
uspto-grants-1995_05
特許番号
US05420134

関連ノート

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