HCID 59457665、化合物 → HCID 59457731、化合物

HRID 418684ノート

反応式

HRID 418684 の反応式
[F:1][C:2]1[CH:30]=[C:29]([N+:31]([O-:33])=[O:32])[CH:28]=[CH:27][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]2[CH:11]=[C:12]([C:14]3[CH2:19][CH2:18][N:17](C(OC(C)(C)C)=O)[CH2:16][CH:15]=3)[S:13][C:6]=12>C(Cl)Cl>[F:1][C:2]1[CH:30]=[C:29]([N+:31]([O-:33])=[O:32])[CH:28]=[CH:27][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]2[CH:11]=[C:12]([C:14]3[CH2:19][CH2:18][NH:17][CH2:16][CH:15]=3)[S:13][C:6]=12

参加物

3

反応物 1

HCID 59457665HCID 59457665、化合物

生成物 1

HCID 59457731HCID 59457731、化合物収率 100%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of tert-butyl 4-(7-(2-fluoro-4-nitrophenoxy)thieno[3,2-b]pyridin-2-yl)-5,6-dihydropyridine-1(2H)-carboxylate 267 (1 g, 2.13 mmol) in DCM (4.3 mL) TFA (4.3 mL) was added and the reaction mixture was stirred for 2 h at room temperature. The solvent was removed under reduced pressure, the residue was suspended in aqueous sodium bicarbonate, the mixture extracted with DCM, EtOAc and DCM; the combined organic phases were filtered and the recovered solids dried. The organic phase was dried over anhydrous Na2SO4, concentrated under reduced pressure and the residue was combined with the solid material obtained earlier to provide 268 (806 mg, 2.12 mmol, 100% yield) as a yellow solid. MS (m/z): (M+1) 372.1 (100%).

後処理

  1. customThe solvent was removed under reduced pressure
  2. extractionthe mixture extracted with DCM, EtOAc and DCM
  3. filtrationthe combined organic phases were filtered
  4. customthe recovered solids dried
  5. dry with materialThe organic phase was dried over anhydrous Na2SO4
  6. concentrationconcentrated under reduced pressure
  7. customobtained earlier

出典と根拠

ORDレコード
ord-97658b1d5ebf47a2a3d51808a9088cd9
出典データセット
uspto-grants-2012_01
特許番号
US08093264B2

反応ノート

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