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

HRID 1156197노트

반응식

HRID 1156197 반응식
[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]

참가 물질

3

반응물 2

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

생성물 1

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

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-07edd047e7f9456287c19ee4838d8d9b
출처 데이터셋
uspto-grants-1982_06
특허 번호
US04334088

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