반응식
[C:1]([OH:10])(=[O:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[NH2:4].[C:11]1([CH3:21])[CH:16]=[CH:15][C:14]([S:17](Cl)(=[O:19])=[O:18])=[CH:13][CH:12]=1.[OH-].[Na+].Cl>O>[S:17]([NH:4][C:3]1[C:2](=[CH:8][CH:7]=[CH:6][CH:5]=1)[C:1]([OH:10])=[O:9])([C:14]1[CH:15]=[CH:16][C:11]([CH3:21])=[CH:12][CH:13]=1)(=[O:19])=[O:18]참가 물질
반응 조건
- 온도
- 75 °C
실험 절차
99.26 g of anthranilic acid was added to 830 g of water, the resulting mixture was heated at 75° C. and 165.3 g of p-toluenesulfonyl chloride was added thereto over 30 minutes with stirring. 495 g of 28% aqueous solution of sodium hydroxide was added dropwise and the mixture was stirred at 80° C. for one hour. The reaction mixture was added dropwise to a mixed solution of 360 g of 35% hydrochloric acid and 270 g of water at 70 to 80° C. and stirred for one hour. After cooling to 30° C., the mixture was filtered, the resulting crystals were washed with water, and the wet crystals were heated and solved in 750 g of 1-propanol to obtain a solution. After cooling to a room temperature, the solution was filtered, the resulting crystals were washed with 1-propanol, and dried under a reduced pressure to obtain 175 g of N-tosyl anthranilic acid.
후처리
- stirringthe mixture was stirred at 80° C. for one hour
- stirringstirred for one hour
- temperatureAfter cooling to 30° C.
- filtrationthe mixture was filtered
- washthe resulting crystals were washed with water
- temperaturethe wet crystals were heated
- customto obtain a solution
- temperatureAfter cooling to a room temperature
- filtrationthe solution was filtered
- washthe resulting crystals were washed with 1-propanol
- customdried under a reduced pressure
출처 및 근거
- ORD 기록
- ord-d6b42f002bf04ae1b1cd8f19a1bb7b9e
- 출처 데이터셋
- uspto-grants-2005_02
- 특허 번호
- US06852862B2
연결된 노트
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