Water → HCID 86665397, 화합물

HRID 2403039노트

반응식

HRID 2403039 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[O:11][CH3:12])[C:5]([NH2:7])=[O:6].C([N:21]=[C:22]=[S:23])(=O)C1C=CC=CC=1.O>CC(C)=O>[CH3:12][O:11][C:10]1[CH:9]=[CH:8][C:4]([C:5]([NH2:7])=[O:6])=[CH:3][C:2]=1[NH:1][C:22]([NH2:21])=[S:23]

참가 물질

5

반응물 3

HCID 962WaterHCID 68284Benzoyl isothiocyanateHCID 871353-Amino-4-methoxybenzamide

생성물 1

HCID 86665397HCID 86665397, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To a solution of 3-amino-4-methoxybenzamide (2.49 g, 15.0 mmol, Alfa) in acetone (30 mL) at reflux was added benzoyl isothiocyanate (2.22 mL, 16.5 mmol) and the mixture was stirred at reflux for 30 min, then was poured into water. The precipitate was collected by vacuum filtration and was treated with 10% aq. NaOH (15 mL). The mixture was heated to reflux for 40 min, cooled to room temperature, and poured into a mixture of ice and 6 N aq. HCl. The mixture was basified to pH 10 with conc. aq. NH4OH and the resulting white solid precipitate was collected by vacuum filtration, affording the crude title compound, which was used without further purification.

후처리

  1. temperatureat reflux for 30 min
  2. filtrationThe precipitate was collected by vacuum filtration
  3. additionwas treated with 10% aq. NaOH (15 mL)
  4. temperatureThe mixture was heated
  5. temperatureto reflux for 40 min
  6. additionpoured into a mixture of ice and 6 N aq. HCl
  7. filtrationthe resulting white solid precipitate was collected by vacuum filtration

출처 및 근거

ORD 기록
ord-0c862289ade24c6b860ecf39410e49bf
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08798939B2

반응 노트

불러오는 중…