Acetonitrile → HCID 2794456、化合物

HRID 2304563ノート

反応式

HRID 2304563 の反応式
[CH2:1]([CH:3]([C:7](Cl)=[O:8])[C:4](Cl)=[O:5])[CH3:2].N[CH2:11][C:12]([C:14]1C=CC=C[CH:15]=1)=O.C([N:22]([CH2:25][CH3:26])CC)C.CC[O-:29].[Na+].[C:31](#N)[CH3:32]>>[CH3:2][C:1]1[C:26]2[C:25](=[CH:11][CH:12]=[CH:14][CH:15]=2)[NH:22][C:4](=[O:5])[C:3]=1[C:7]([O:8][CH2:31][CH3:32])=[O:29]

参加物

6

反応物 5

HCID 6342Acetonitrile2 回HCID 8471TriethylamineHCID 11952PhenacylamineHCID 2723922Sodium ethoxideHCID 109209242-Ethylpropanedioyl dichloride

生成物 1

HCID 2794456HCID 2794456、化合物収率 84%

実験手順

A solution of ethylmalonyl chloride (12.9 ml, 100 mmol) in anhydrous acetonitrile (30 ml) is added dropwise to a solution of 2-aminoacetophenone (10.5 g, 78 mmol) and triethylamine (13.9 ml, 100 mmol) in anhydrous acetonitrile (110 ml), under argon and at 0° C. The reaction medium is heated up to ambient temperature then treated dropwise and under argon with a solution of sodium ethylate (obtained with 1.8 g, 78 mmol, of sodium in 80 ml of ethanol), then left under agitation for 12 hours at ambient temperature. The reaction mixture is then poured into ice cold water (100 ml) and agitated for two hours, then filtered. The precipitate collected in this way is washed with water, with ethanol and with ether in order to produce 15.2 g (84%) of a white solid.

後処理

  1. filtrationfiltered
  2. customThe precipitate collected in this way
  3. washis washed with water, with ethanol and with ether in order

出典と根拠

ORDレコード
ord-94acfff982c3403a873a8081385409de
出典データセット
uspto-grants-2002_08
特許番号
US06436951B1

反応ノート

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