Water → HCID 22238083、化合物

HRID 1743386ノート

反応式

HRID 1743386 の反応式
[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]

参加物

6

反応物 4

HCID 962WaterHCID 112413-Chloro-2-methyl-1-propeneHCID 11430Potassium CarbonateHCID 22238064HCID 22238064、化合物

生成物 1

HCID 22238083HCID 22238083、化合物収率 96.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0349468f72964b50bd23b8bd76089e4a
出典データセット
uspto-grants-2006_03
特許番号
US07008940B1

反応ノート

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