Ethanol hydrochloride → 1-Acetyl-3-(2-ethoxycarbonylethyl)-4,6-dimethylindoline

HRID 1531972노트

반응식

HRID 1531972 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]([OH:19])=[O:18])[CH2:5]1)(=[O:3])[CH3:2].Cl.[CH3:21][CH2:22]O>CCO>[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][CH2:21][CH3:22])=[O:18])[CH2:5]1)(=[O:3])[CH3:2]

참가 물질

4

반응물 2

HCID 21887872Ethanol hydrochlorideHCID 222473451-Acetyl-3-(2-carboxyethyl)-4,6-dimethylindoline

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

1-Acetyl-3-(2-carboxyethyl)-4,6-dimethylindoline (3.4 g) was dissolved in EtOH (50 ml) and 10N HCl-EtOH (3.9 ml) was added, which was followed by refluxing for 30 min. EtOH was evaporated under reduced pressure and AcOEt (100 ml) was added. After washing with water, the mixture was dried over anhydrous sodium sulfate. AcOEt was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: CHCl3/MeOH=50/1−10/1) to give 3.3 g of 1-acetyl-3-(2-ethoxycarbonylethyl)-4,6-dimethylindoline.

후처리

  1. temperatureby refluxing for 30 min
  2. customEtOH was evaporated under reduced pressure and AcOEt (100 ml)
  3. additionwas added
  4. washAfter washing with water
  5. dry with materialthe mixture was dried over anhydrous sodium sulfate
  6. customAcOEt 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-d98a421356e34045b8d0b47f7011db50
출처 데이터셋
uspto-grants-2001_03
특허 번호
US06200988B1

반응 노트

불러오는 중…