3-Methylbenzoic acid → 3-Methylbenzoyl chloride

HRID 37185

반응식

HRID 37185 반응식
[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]

참가 물질

5

반응물 2

HCID 74183-Methylbenzoic acidHCID 65578Oxalyl chloride

생성물 1

HCID 743753-Methylbenzoyl chloride

시약·촉매·용매 2

HCID 6228Dimethylformamide촉매HCID 241Benzene용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-327c30f17ea74844a93444c148790f2c
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05420134

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