Tetrahydrofuran → HCID 178477272, 화합물

HRID 533668

반응식

HRID 533668 반응식
[NH2:1][C:2]1[C:3]([OH:12])=[N:4][CH:5]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1.C1COCC1.Cl.[CH2:19]([S:21][C:22]1[CH:30]=[CH:29][CH:28]=[CH:27][C:23]=1[C:24](O)=[O:25])[CH3:20].C(=O)([O-])O.[Na+]>O>[CH2:19]([S:21][C:22]1[CH:30]=[CH:29][CH:28]=[CH:27][C:23]=1[C:24]([NH:1][C:2]1[C:3]([OH:12])=[N:4][CH:5]=[C:6]([C:8]([F:11])([F:9])[F:10])[CH:7]=1)=[O:25])[CH3:20]

참가 물질

6

반응물 4

HCID 8028TetrahydrofuranHCID 516892Sodium BicarbonateHCID 23157873-Amino-5-(trifluoromethyl)-1,2-dihydropyridin-2-oneHCID 679812702-Ethylsulfanylbenzoic acid hydrochloride

생성물 1

HCID 178477272HCID 178477272, 화합물수율 95%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a mixture of 3-amino-5-trifluoromethylpyridin-2-ol (0.75 g) and THF (5 ml), 2-ethylsulfanylbenzoic acid hydrochloride (0.93 g) was added under ice-cooling, heated to room temperature, and stirred for 2 hours. After the mixture was allowed to stand overnight, the mixture was heated to 50° C., and stirred with heating for 6 hours. To the mixture, sodium hydrogen carbonate (0.35 g) was added, and stirred with heating for further 2.5 hours. After the mixture was allowed to stand, water was poured thereinto, and the precipitated solid was collected by filtration. The obtained solid was washed with water, and dried to give 1.37 g of 2-ethylsulfanyl-N-(2-hydroxy-5-trifluoromethylpyridin-3-yl)-benzamide (Compound (1B)-506).

후처리

  1. additionwas added under ice-
  2. temperaturecooling
  3. waitto stand overnight
  4. temperaturethe mixture was heated to 50° C.
  5. stirringstirred
  6. temperaturewith heating for 6 hours
  7. stirringstirred
  8. temperaturewith heating for further 2.5 hours
  9. filtrationthe precipitated solid was collected by filtration
  10. washThe obtained solid was washed with water
  11. customdried

출처 및 근거

ORD 기록
ord-749b48b601664bd183c36e0ad08f3ea7
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08853238B2

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