Oxalyl chloride → 2,3-Dihydro-1-benzofuran-7-carbonyl chloride

HRID 1533055

반응식

HRID 1533055 반응식
[O:1]1[CH2:5][CH2:4][C:3]2[CH:6]=[CH:7][CH:8]=[C:9]([C:10]([OH:12])=O)[C:2]1=2.C(Cl)(=O)C([Cl:16])=O>ClCCl.CN(C)C=O>[O:1]1[CH2:5][CH2:4][C:3]2[CH:6]=[CH:7][CH:8]=[C:9]([C:10]([Cl:16])=[O:12])[C:2]1=2

참가 물질

5

반응물 2

HCID 65578Oxalyl chlorideHCID 27950142,3-Dihydro-1-benzofuran-7-carboxylic acid

생성물 1

HCID 27950162,3-Dihydro-1-benzofuran-7-carbonyl chloride수율 98.9%

시약·촉매·용매 2

HCID 6228Dimethylformamide촉매HCID 6344Dichloromethane용매

실험 절차

2,3-Dihydrobenzo[b]furan-7-oic acid (3 g) (see Preparation 32) was suspended in anhydrous dichloromethane (30 ml) and oxalyl chloride (3.5 g) added, followed by addition of dimethylformamide (3 drops). The mixture was stirred at room temperature for 2.5 hours, the solvent then removed under reduced pressure, the resulting residue dissolved in dichloromethane and the solvent removed under reduced pressure. The residue was again dissolved in dichloromethane and the solvent removed under reduced pressure to give 2,3-dihydrobenzo[b]furan-7-oyl chloride as a pink solid (3.3 g).

후처리

  1. customthe solvent then removed under reduced pressure
  2. dissolutionthe resulting residue dissolved in dichloromethane
  3. customthe solvent removed under reduced pressure
  4. dissolutionThe residue was again dissolved in dichloromethane
  5. customthe solvent removed under reduced pressure

출처 및 근거

ORD 기록
ord-9642afae95fe480ab07f43aa4726d067
출처 데이터셋
uspto-grants-2001_03
특허 번호
US06207678B1

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