Water → HCID 22238083, 화합물

HRID 1743386노트

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HRID 1743386 반응식
[OH:1][C:2]1[CH:3]=[C:4]2[C:8](=[C:9]([CH3:12])[C:10]=1[CH3:11])[N:7]([CH:13]=[O:14])[CH:6]([CH3:15])[CH2:5]2.Cl[CH2:17][C:18]([CH3:20])=[CH2:19].C(=O)([O-])[O-].[K+].[K+].O>CN(C=O)C>[CH3:15][CH:6]1[CH2:5][C:4]2[C:8](=[C:9]([CH3:12])[C:10]([CH3:11])=[C:2]([O:1][CH2:19][C:18]([CH3:20])=[CH2:17])[CH:3]=2)[N:7]1[CH:13]=[O:14]

참가 물질

6

반응물 4

HCID 962WaterHCID 112413-Chloro-2-methyl-1-propeneHCID 11430Potassium CarbonateHCID 22238064HCID 22238064, 화합물

생성물 1

HCID 22238083HCID 22238083, 화합물수율 96.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
60 °C

실험 절차

A suspension of 2,3-dihydro-5-hydroxy-2,6,7-trimethyl-1H-indole-1-carbaldehyde (0.5 g, 2.4 mmol), 3-chloro-2-methyl-1-propene (0.29 mL, 2.9 mmol) and potassium carbonate (0.50 g, 3.6 mmol) in DMF (6 mL) was stirred at 60° C. for 14 hours under the nitrogen atmosphere. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate two times. The combined organic layers were washed with water and saturated brine, dried over magnesium sulfate, filtered, and concentrated under reduced pressure. The residue was subjected to silica gel columns chromatography (hexane-ethyl acetate 3:1) to obtain 0.60 g of the title compound.

후처리

  1. extractionthe mixture was extracted with ethyl acetate two times
  2. washThe combined organic layers were washed with water and saturated brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-0349468f72964b50bd23b8bd76089e4a
출처 데이터셋
uspto-grants-2006_03
특허 번호
US07008940B1

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