Acetic Anhydride → 2,3-Dichloro-4-(2-phenylacryloyl)anisole

HRID 1156197ノート

反応式

HRID 1156197 の反応式
[Cl:1][C:2]1[C:7]([Cl:8])=[C:6]([C:9](=[O:17])[CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:5]=[CH:4][C:3]=1[O:18][CH3:19].[C:20](OC(=O)C)(=O)C>>[Cl:1][C:2]1[C:7]([Cl:8])=[C:6]([C:9](=[O:17])[C:10]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH2:20])[CH:5]=[CH:4][C:3]=1[O:18][CH3:19]

参加物

3

反応物 2

HCID 7918Acetic AnhydrideHCID 111301952,3-Dichloro-4-phenylacetylanisole

生成物 1

HCID 109248102,3-Dichloro-4-(2-phenylacryloyl)anisole収率 94%

実験手順

Acetic anhydride (150 ml.) is added dropwise to a suspension of 2,3-dichloro-4-phenylacetylanisole (8.95 g., 30.3 mmol) in 15.3 ml. of N,N,N'N'-tetramethylenediaminomethane under an atmosphere of argon with icebath cooling. The reaction mixture stirred at 25° for 2 hrs. and poured into ice-water affords 11.9 g. of beige solid. An ethereal solution of the solid is washed with hydrochloric acid, water and then dried over magnesium sulfate. Removal of the solvent under reduced pressure provides 8.77 g. (94% yield) of 2,3-dichloro-4-(2-phenylacryloyl)anisole, m.p. 83.5°-86°.

後処理

  1. customaffords 11.9 g
  2. washAn ethereal solution of the solid is washed with hydrochloric acid, water
  3. dry with materialdried over magnesium sulfate
  4. customRemoval of the solvent under reduced pressure
  5. customprovides 8.77 g

出典と根拠

ORDレコード
ord-07edd047e7f9456287c19ee4838d8d9b
出典データセット
uspto-grants-1982_06
特許番号
US04334088

反応ノート

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