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Acetic Acid → HCID 21464431、化合物

HRID 1898834
ノート
印刷プレビュー

反応式

HRID 1898834 の反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[NH:9][S:10]([C:13]1[N:24]=[C:16]2[C:17]([O:22][CH3:23])=[CH:18][CH:19]=[C:20](Cl)[N:15]2[N:14]=1)(=[O:12])=[O:11].C[O-].[Na+].CS(C)=O.[C:32](O)(=[O:34])C>ClCCl.O>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[NH:9][S:10]([C:13]1[N:24]=[C:16]2[C:17]([O:22][CH3:23])=[CH:18][CH:19]=[C:20]([O:34][CH3:32])[N:15]2[N:14]=1)(=[O:12])=[O:11]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 176Acetic AcidHCID 679Dimethyl SulfoxideHCID 10942334Sodium MethoxideHCID 21464366HCID 21464366、化合物

生成物 1

HCID 21464431HCID 21464431、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6344
Dichloromethane
溶媒

反応条件

温度
70 °C

実験手順

N-(2,6-Difluorophenyl)-5-chloro-8-methoxy[1,2,4]triazolo[1,5-a]pyridine-2-sulfonamide (1.0 g, 2.7 mmol), sodium methoxide (25 percent in methanol, 2.5 mL, 0.58 g, 11 mmol) and dimethyl sulfoxide (20 mL) were mixed with stirring and slowly heated to 70° C. over a 40-min period. After a short reaction period, the reaction mixture was acidified with acetic acid and diluted With dichloromethane and water. The solid that separated was recovered by filtration. The organic layer was separated, was washed several times with water, and was concentrated by evaporation under reduced pressure. The residue obtained was washed with water and combined with the previously obtained solid. The combined solids were washed with ether and hexane and dried to obtain 0.7 g of the title compound as an off-white powder melting at 319°-320° C.(d).

後処理

  1. customAfter a short reaction period
  2. customThe solid that separated
  3. filtrationwas recovered by filtration
  4. customThe organic layer was separated
  5. washwas washed several times with water
  6. concentrationwas concentrated by evaporation under reduced pressure
  7. customThe residue obtained
  8. washwas washed with water
  9. washThe combined solids were washed with ether and hexane
  10. customdried

出典と根拠

ORDレコード
ord-5a65190be1f4415399dd2f5108542650
出典データセット
uspto-grants-1996_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05571775

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート