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Trifluoroacetic acid → HCID 57671538、化合物

HRID 1801990
ノート
印刷プレビュー

反応式

HRID 1801990 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]([NH:12][CH3:13])=[CH:10][N:11]=1)[C:5]([O:7]C)=O.[C:14]([O:18][C:19]([C:21]1[C:26](C(OC)=O)=CC(Cl)=NC=1)=[O:20])(C)(C)C.C(O)(C(F)(F)F)=[O:33]>C(Cl)Cl>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][N:11]=1)[N:12]([CH3:13])[C:26](=[O:33])[C:21]([C:19]([O:18][CH3:14])=[O:20])=[C:5]2[OH:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 57671617HCID 57671617、化合物HCID 86631269HCID 86631269、化合物

生成物 1

HCID 57671538HCID 57671538、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Methyl 2-chloro-5-(methylamino)isonicotinate. To a solution of methyl 5-(tert-butoxycarbonyl)-2-chloroisonicotinate (0.5 g, 1.7 mmol) in dry DCM (10 mL) was added TFA (4.4 mL) with stirring and cooling using an ice-bath. The mixture was stirred at room temperature for 2 hours and then evaporated under reduced pressure. The residue was dissolved in water, and the solution was adjusted to pH=8 by treatment with saturated NaHCO3. The mixture was extracted twice with EtOAc. The combined organic layers were dried over anhydrous MgSO4, and filtered. The filtrate was evaporated under reduced pressure, and the residue was dried in vacuo to give the title compound.

後処理

  1. temperaturecooling
  2. stirringThe mixture was stirred at room temperature for 2 hours
  3. customevaporated under reduced pressure
  4. dissolutionThe residue was dissolved in water
  5. extractionThe mixture was extracted twice with EtOAc
  6. dry with materialThe combined organic layers were dried over anhydrous MgSO4
  7. filtrationfiltered
  8. customThe filtrate was evaporated under reduced pressure
  9. customthe residue was dried in vacuo

出典と根拠

ORDレコード
ord-f27b3c908d9f455395190c591d0e0a4c
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08349868B2

反応ノート

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