Hydrochloric Acid → Benzamide, 2-(benzoyloxy)-N-(4-(benzoyloxy)-3,5-dichlorophenyl)-

HRID 1282947노트

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HRID 1282947 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:15]=[C:16]([Cl:19])[C:17]=1[OH:18])[NH:5][C:6](=[O:14])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[OH:13].[C:20](Cl)(=[O:27])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.Cl>N1C=CC=CC=1>[C:20]([O:13][C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=1[C:6]([NH:5][C:4]1[CH:3]=[C:2]([Cl:1])[C:17]([O:18][C:6](=[O:14])[C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[C:16]([Cl:19])[CH:15]=1)=[O:14])(=[O:27])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 7412Benzoyl chlorideHCID 10424739HCID 10424739, 화합물

생성물 1

HCID 3043339Benzamide, 2-(benzoyloxy)-N-(4-(benzoyloxy)-3,5-dichlorophenyl)-수율 88.2%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

3',5'-Dichloro-2,4'-dihydroxybenzanilide (1 g.) was dissolved in dry pyridine (15 ml.) in the cold at 0°- 5° C. and to it was added dropwise benzoyl chloride (1.2 ml.). With gentle stirring reaction was continued for several hours. The solution was then poured into ice-cold water and acidified with 1 N hydrochloric acid to pH 2, yielding oily material which was extracted by ethyl acetate. The ethyl acetate solution was washed with 1 N hydrochloric acid and 5% sodium bicarbonate solution in that order and dried with anhydrous sodium sulfate, followed by removal of the solvent by evaporation. The residue was subjected to recrystallization from ether and petroleum ether mixture to give white crystals (1.5 g.) of 2,4'-dibenzoyloxy-3',5'-dichlorobenzanilide. Yield: 88.2%. Melting point: 157°-160° C.

후처리

  1. customreaction
  2. waitwas continued for several hours
  3. additionThe solution was then poured into ice-cold water
  4. customyielding oily material which
  5. extractionwas extracted by ethyl acetate
  6. washThe ethyl acetate solution was washed with 1 N hydrochloric acid and 5% sodium bicarbonate solution in that order
  7. dry with materialdried with anhydrous sodium sulfate
  8. customfollowed by removal of the solvent by evaporation
  9. customThe residue was subjected to recrystallization from ether and petroleum ether mixture

출처 및 근거

ORD 기록
ord-d02f8d5cd56b4eb1827fed8f2103a123
출처 데이터셋
uspto-grants-1976_08
특허 번호
US03973038

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