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Water → HCID 18509279, 화합물

HRID 1356638
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HRID 1356638 반응식
[Cl:1][C:2]1[CH:19]=[CH:18][C:5]([N:6]([CH3:17])[S:7]([C:10]2[CH:15]=[CH:14][C:13]([CH3:16])=[CH:12][CH:11]=2)(=[O:9])=[O:8])=[C:4]([C:20](=O)[NH2:21])[CH:3]=1.FC(F)(F)C(OC(=O)C(F)(F)F)=O.O>N1C=CC=CC=1>[Cl:1][C:2]1[CH:19]=[CH:18][C:5]([N:6]([CH3:17])[S:7]([C:10]2[CH:11]=[CH:12][C:13]([CH3:16])=[CH:14][CH:15]=2)(=[O:8])=[O:9])=[C:4]([C:20]#[N:21])[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 9845Trifluoroacetic anhydrideHCID 18509237HCID 18509237, 화합물

생성물 1

HCID 18509279HCID 18509279, 화합물수율 95%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

To a solution of 4′-chloro-2′-carbamoyl-N-methyl-p-toluenesulfonanilide (0.70 g (2.07 mmol)) in pyridine (3.0 ml), under cooling with ice and with stirring, trifluoroacetic anhydride (0.40 ml (2.83 mmol)) was added dropwise. The temperature of the reaction mixture was brought to room temperature and the mixture was stirred at the same temperature for 2 hours. Then, the mixture was poured into water and extracted with ethyl acetate. The extract was washed with dilute hydrochloric acid, water and saturated sodium chloride solution, successively, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. Diisopropyl ether was added to the residue and crystals separated was filtered and washed to give 0.63 g (95%) of the title compound as white crystals.

후처리

  1. customwas brought to room temperature
  2. stirringthe mixture was stirred at the same temperature for 2 hours
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with dilute hydrochloric acid, water and saturated sodium chloride solution
  5. dry with materialsuccessively, dried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. additionDiisopropyl ether was added to the residue and crystals
  8. customseparated
  9. filtrationwas filtered
  10. washwashed

출처 및 근거

ORD 기록
ord-c94b7d49e8514ded80ee6e9136dc5a1d
출처 데이터셋
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06586617B1

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