Chlorodifluoromethane → HCID 69898430、化合物

HRID 1884220ノート

反応式

HRID 1884220 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][CH2:12][NH:13][C:14](=[O:25])[C:15]([C:18]2[CH:23]=[CH:22][C:21]([CH3:24])=[CH:20][CH:19]=2)=[CH:16][OH:17])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[OH-].[K+].Cl[CH:29]([F:31])[F:30]>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.COCCOC>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][CH2:12][NH:13][C:14](=[O:25])[C:15]([C:18]2[CH:23]=[CH:22][C:21]([CH3:24])=[CH:20][CH:19]=2)=[CH:16][O:17][CH:29]([F:31])[F:30])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

参加物

6

反応物 3

HCID 6372ChlorodifluoromethaneHCID 14797Potassium Hydroxide2 回HCID 69898186HCID 69898186、化合物

生成物 1

HCID 69898430HCID 69898430、化合物

試薬・触媒・溶媒 2

HCID 74236Tetrabutylammonium Bromide触媒HCID 80711,2-Dimethoxyethane溶媒

実験手順

Five hundred milligrams (500 mg) of N-[2-(3,4-dimethoxyphenyl)ethyl]-3-hydroxy-2-(4-methylphenyl)acrylamide (1.46 mmol), 0.31 g (1.7 mmol) of 30% aqueous potassium hydroxide solution, 0.1 g (0.3 mmol) of tetrabutylammonium bromide and 10 ml of ethylene glycol dimethyl ether were mixed and chlorodifluoromethane gas was blown thereto at room temperature. After a small amount of 30% aqueous potassium hydroxide solution was further added, a sample was taken out from the reaction mixture and the disappearance of the starting material was confirmed by thin layer chromatograph analysis. Then, 5% hydrochrolic acid was added to the reaction mixture, which was followed by extracted with ethyl acetate, washed with 5% hydrochrolic acid, saturated aqueous sodium bicarbonate solution and saturated brine subsequently, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was washed with hexane to give 474 mg of N-[2-(3,4-dimethoxyphenyl) ethyl]-3-difluoromethoxy-2-(4-methylphenyl)acrylamide (the present compound 1005).

後処理

  1. customat room temperature
  2. extractionby extracted with ethyl acetate
  3. washwashed with 5% hydrochrolic acid, saturated aqueous sodium bicarbonate solution and saturated brine subsequently
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. washThe residue was washed with hexane

出典と根拠

ORDレコード
ord-b84830c6142c46ccb9f988b6667f8638
出典データセット
uspto-grants-2004_07
特許番号
US06762321B2

反応ノート

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