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Potassium Iodide → HCID 15034422、化合物

HRID 1073854
ノート
印刷プレビュー

反応式

HRID 1073854 の反応式
C([O:3][CH:4](OCC)[CH2:5][O:6][C:7]1[CH:12]=[C:11]([F:13])[CH:10]=[CH:9][C:8]=1[O:14][CH3:15])C.FC1C=CC(OC)=C(O)C=1.C(=O)([O-])[O-].[K+].[K+].C(OC(OCC)CCl)C.[I-].[K+]>CN(C)C=O>[F:13][C:11]1[CH:10]=[CH:9][C:8]([O:14][CH3:15])=[C:7]([CH:12]=1)[O:6][CH2:5][CH:4]=[O:3]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 121282-Chloro-1,1-diethoxyethaneHCID 27745595-Fluoro-2-methoxyphenolHCID 15079980HCID 15079980、化合物

生成物 1

HCID 15034422HCID 15034422、化合物

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

反応条件

温度
100 °C

実験手順

2-(5-Fluoro-2-methoxyphenoxy)acetaldehyde diethylacetal A suspension of 10.8 g of 5-fluoro-2-methoxyphenol and 12.6 g of potassium carbonate in 45 ml of N,N-dimethylformamide was heated for 45 minutes at 100° C. To the reaction mixture were added 18.5 ml of chloroacetaldehyde diethylacetal and 12.7 g of potassium iodide and the reaction mixture was heated for 4 hours at 140° C. After cooling, the reaction mixture was poured into ice water and extracted with ether. The extract was washed with aqueous sodium hydroxide solution and water, dried and evaporated. The residue was chromatographed on silica gel using chloroform as an eluant to give 11.8 g of the desired compound as a colorless oil.

後処理

  1. temperaturethe reaction mixture was heated for 4 hours at 140° C
  2. temperatureAfter cooling
  3. extractionextracted with ether
  4. washThe extract was washed with aqueous sodium hydroxide solution and water
  5. customdried
  6. customevaporated
  7. customThe residue was chromatographed on silica gel

出典と根拠

ORDレコード
ord-89ee9849da724acf9d058f4a23d96a48
出典データセット
uspto-grants-1990_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04971990

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート