Tetrahydrofuran → HCID 178477272、化合物

HRID 533668

反応式

HRID 533668 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 178477272HCID 178477272、化合物収率 95%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-749b48b601664bd183c36e0ad08f3ea7
出典データセット
uspto-grants-2014_10
特許番号
US08853238B2

関連ノート

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