Acetic Anhydride → HCID 58747567, 화합물

HRID 2378366노트

반응식

HRID 2378366 반응식
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

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 81531DiisopropylethylamineHCID 86608751HCID 86608751, 화합물

생성물 1

HCID 58747567HCID 58747567, 화합물수율 66.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

[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.

후처리

  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

출처 및 근거

ORD 기록
ord-49516bdfb6f645acb739328ef46cd4e0
출처 데이터셋
uspto-grants-2008_12
특허 번호
US07470799B2

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