Iodoethane → HCID 22490930、化合物

HRID 2180598ノート

反応式

HRID 2180598 の反応式
[Br:1][C:2]1[C:11]2[C:10]([CH3:13])([CH3:12])[CH2:9][CH:8]=[C:7]([CH:14]([CH3:16])[CH3:15])[C:6]=2[CH:5]=[C:4]([C:17](=[O:19])[CH3:18])[C:3]=1[OH:20].C(=O)([O-])[O-].[K+].[K+].[CH2:27](I)[CH3:28]>CC(C)=O.O>[Br:1][C:2]1[C:11]2[C:10]([CH3:13])([CH3:12])[CH2:9][CH:8]=[C:7]([CH:14]([CH3:16])[CH3:15])[C:6]=2[CH:5]=[C:4]([C:17](=[O:19])[CH3:18])[C:3]=1[O:20][CH2:27][CH3:28]

参加物

6

反応物 3

HCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 22490824HCID 22490824、化合物

生成物 1

HCID 22490930HCID 22490930、化合物

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 962Water溶媒

実験手順

A mixture of 1-(4-bromo-3-hydroxy-8-isopropyl-5,5-dimethyl-5,6-dihydro-naphthalen-2-yl)-ethanone (Compound A-106, 1.61 g, 4.77 mmol), potassium carbonate (1.97 g, 14.31 mmol) and ethyl iodide (3.8 mL, 47.7 mmol) in acetone (50 mL) was heated to reflux for 16 h. The reaction mixture was cooled to room temperature, diluted with water and extracted with diethyl ether. The combined ethereal layers were washed with water, brine, dried (Na2SO4), filtered and concentrated in vacuo to give the title compound as a yellow oil. The material was used in the next step without further purification.

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 16 h
  3. extractionextracted with diethyl ether
  4. washThe combined ethereal layers were washed with water, brine
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-e36bccdb2ee3477bb6b30a953db54f02
出典データセット
uspto-grants-2005_05
特許番号
US06887896B1

反応ノート

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