Potassium Carbonate → 6-(Pentyloxy)-2h-3-chromenecarbaldehyde

HRID 394696

反応式

HRID 394696 の反応式
[OH:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[O:8][CH2:7][C:6]([CH:12]=[O:13])=[CH:5]2.I[CH2:15][CH2:16][CH2:17][CH2:18][CH3:19].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH2:15]([O:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[O:8][CH2:7][C:6]([CH:12]=[O:13])=[CH:5]2)[CH2:16][CH2:17][CH2:18][CH3:19]

参加物

5

反応物 3

HCID 11430Potassium Carbonate2 回HCID 123351-IodopentaneHCID 47708156-Hydroxychromene-3-carboxaldehyde

生成物 1

HCID 181774176-(Pentyloxy)-2h-3-chromenecarbaldehyde

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

2 g (11.4 mmol) of the hydroxyaldehyde obtained in Step A and also 2.7 g (13.6 mmol) of iodopentane are added to a suspension of 1.9 g (13.6 mmol) of potassium carbonate in 50 ml of anhydrous acetone; the medium is then heated at reflux. After one hour, 1.2 g of potassium carbonate are added to the solution, and that operation is then re-started after one hour. At the end of 12 hours of heating at reflux, the solution is allowed to cool, the salts are filtered off over Celite and the solvent is then evaporated in vacuo. Chromatography on a silica column (eluant: petroleum ether/ethyl acetate 90/10) yields the title aldehyde in the form of a yellow syrup.

後処理

  1. temperaturethe medium is then heated
  2. temperatureat reflux
  3. waitre-started after one hour
  4. temperatureAt the end of 12 hours of heating
  5. temperatureat reflux
  6. temperatureto cool
  7. filtrationthe salts are filtered off over Celite
  8. customthe solvent is then evaporated in vacuo

出典と根拠

ORDレコード
ord-7b2eb4b6957743e1a13dfd3b486b8b36
出典データセット
uspto-grants-2003_08
特許番号
US06602903B2

関連ノート

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