Formic Acid → HCID 20397149, 화합물

HRID 462766노트

반응식

HRID 462766 반응식
[C:1](OC(=O)C)(=[O:3])C.C(O)=O.[NH2:11][C:12]1[C:17]([Cl:18])=[CH:16][C:15]([NH:19][C:20](=[O:25])[C:21]([Cl:24])([Cl:23])[Cl:22])=[CH:14][C:13]=1[Cl:26]>>[Cl:26][C:13]1[CH:14]=[C:15]([NH:19][C:20](=[O:25])[C:21]([Cl:24])([Cl:22])[Cl:23])[CH:16]=[C:17]([Cl:18])[C:12]=1[NH:11][CH:1]=[O:3]

참가 물질

4

반응물 3

HCID 284Formic AcidHCID 7918Acetic AnhydrideHCID 20397151HCID 20397151, 화합물

생성물 1

HCID 20397149HCID 20397149, 화합물수율 69.1%

반응 조건

온도
5 °C

실험 절차

Acetic anhydride (600 mL, 6.4 mol) and 90% formic acid (275 mL, 5.4 mol) are heated to reflux for 45 minutes and then cooled to 5° C. The N-(4-amino-3,5-dichlorophenyl)-trichloroacetamide (464 g., 1.44 mol) is added to the mixed anhydride solution and mechanically stirred for 20 hours at room temperature. Then the reaction mixture is poured onto ice (2 liters). When the stirred slurry reaches room temperature, it is collected by suction filtration and washed with water (1.5 liters) and dried to constant weight yielding 348.7 grams of N-(3,5-dichloro-4-formamidophenyl)-trichloroacetamide with a mass spectral analysis of m/e+· 348 for C9H5Cl5N2O2.

후처리

  1. temperatureto reflux for 45 minutes
  2. additionThen the reaction mixture is poured onto ice (2 liters)
  3. customreaches room temperature
  4. filtrationit is collected by suction filtration
  5. washwashed with water (1.5 liters)
  6. customdried to constant weight

출처 및 근거

ORD 기록
ord-2aac8e9319aa4392b616a208045e4d8b
출처 데이터셋
uspto-grants-1985_05
특허 번호
US04517199

반응 노트

불러오는 중…