Acetic Anhydride → HCID 58747567、化合物

HRID 2378366ノート

反応式

HRID 2378366 の反応式
Cl.[Cl:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([Cl:9])[C:4]=1[C:10]1[C:18]2[O:17][CH:16](NC)[CH2:15][C:14]=2[CH:13]=[CH:12][CH:11]=1.[CH:21]([N:24]([CH:27](C)C)CC)(C)[CH3:22].C(OC(=O)C)(=[O:32])C>C(Cl)Cl>[Cl:9][C:5]1[CH:6]=[CH:7][CH:8]=[C:3]([Cl:2])[C:4]=1[C:10]1[C:18]2[O:17][CH:16]([CH2:27][NH:24][C:21](=[O:32])[CH3:22])[CH2:15][C:14]=2[CH:13]=[CH:12][CH:11]=1

参加物

5

反応物 3

HCID 7918Acetic AnhydrideHCID 81531DiisopropylethylamineHCID 86608751HCID 86608751、化合物

生成物 1

HCID 58747567HCID 58747567、化合物収率 66.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

[7-(2,6-Dichloro-phenyl)-2,3-dihydro-benzofuran-2-yl]-methylamine hydrochloride (0.050 g, 0.17 mmol) was suspended in 5.0 mL of methylene chloride and diisopropylethylamine (0.072 g, 0.56 mmol) and acetic anhydride (0.029 g, 0.28 mmol) added. The mixture was stirred at room temperature for 30 min, diluted to 100 mL with methylene chloride, washed with 50 mL portions of 2 N HCl (aqueous), saturated aqueous sodium bicarbonate and saturated brine. The solution was dried over sodium sulfate, filtered and concentrated in vacuum to give 0.038 g of the title compound as a white crystalline solid.

後処理

  1. washwashed with 50 mL portions of 2 N HCl (aqueous), saturated aqueous sodium bicarbonate and saturated brine
  2. dry with materialThe solution was dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuum

出典と根拠

ORDレコード
ord-49516bdfb6f645acb739328ef46cd4e0
出典データセット
uspto-grants-2008_12
特許番号
US07470799B2

反応ノート

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