Bromine → 1-Acetyl-5-bromo-3-(2-ethoxycarbonylethyl)-4,6-dimethylindoline

HRID 1107960노트

반응식

HRID 1107960 반응식
[C:1]([N:4]1[C:12]2[C:7](=[C:8]([CH3:14])[CH:9]=[C:10]([CH3:13])[CH:11]=2)[CH:6]([CH2:15][CH2:16][C:17]([O:19][CH2:20][CH3:21])=[O:18])[CH2:5]1)(=[O:3])[CH3:2].[Br:22]Br>CC(O)=O>[C:1]([N:4]1[C:12]2[C:7](=[C:8]([CH3:14])[C:9]([Br:22])=[C:10]([CH3:13])[CH:11]=2)[CH:6]([CH2:15][CH2:16][C:17]([O:19][CH2:20][CH3:21])=[O:18])[CH2:5]1)(=[O:3])[CH3:2]

참가 물질

4

반응물 2

HCID 24408BromineHCID 222473291-Acetyl-3-(2-ethoxycarbonylethyl)-4,6-dimethylindoline

생성물 1

HCID 222473121-Acetyl-5-bromo-3-(2-ethoxycarbonylethyl)-4,6-dimethylindoline

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

1-Acetyl-3-(2-ethoxycarbonylethyl)-4,6-dimethylindoline (3.3 g) was dissolved in AcOH (30 ml) and Br2 (0.93 ml) was added, which was followed by stirring for 30 min. The reaction mixture was poured into ice water and precipitated crude crystals were collected by filtration. The obtained crystals were dissolved in CHCl3 (100 ml). After washing with water, the mixture was dried over anhydrous sodium sulfate. CHCl3 was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: CHCl3 /MeOH=50/1-10/1) to give 3.0 g of 1-acetyl-5-bromo-3-(2-ethoxycarbonylethyl)-4,6-dimethylindoline.

후처리

  1. customprecipitated crude crystals
  2. filtrationwere collected by filtration
  3. dissolutionThe obtained crystals were dissolved in CHCl3 (100 ml)
  4. washAfter washing with water
  5. dry with materialthe mixture was dried over anhydrous sodium sulfate
  6. customCHCl3 was evaporated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (eluent: CHCl3 /MeOH=50/1-10/1)

출처 및 근거

ORD 기록
ord-d2dbdd01f97a456daac93587aabc6ab7
출처 데이터셋
uspto-grants-2000_05
특허 번호
US06063806

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