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

HRID 844573

反応式

HRID 844573 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide触媒HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-1f85b15f8e274e999f0c849357aa9b83
出典データセット
uspto-grants-2002_04
特許番号
US06380396B1

関連ノート

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