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

HRID 1533055

反応式

HRID 1533055 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-9642afae95fe480ab07f43aa4726d067
出典データセット
uspto-grants-2001_03
特許番号
US06207678B1

関連ノート

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