Ammonium Chloride → 4-(2,2-Dioxido-3,4-dihydropyrido[2,1-c][1,2,4]thiadiazin-9-yl)phenol

HRID 1622676

反応式

HRID 1622676 の反応式
CCCC[N+](CCCC)(CCCC)CCCC.[F-].[Si]([O:26][C:27]1[CH:32]=[CH:31][C:30]([C:33]2[C:38]3=[N:39][S:40](=[O:44])(=[O:43])[CH2:41][CH2:42][N:37]3[CH:36]=[CH:35][CH:34]=2)=[CH:29][CH:28]=1)(C(C)(C)C)(C)C.[NH4+].[Cl-]>C1COCC1>[O:44]=[S:40]1(=[O:43])[CH2:41][CH2:42][N:37]2[CH:36]=[CH:35][CH:34]=[C:33]([C:30]3[CH:31]=[CH:32][C:27]([OH:26])=[CH:28][CH:29]=3)[C:38]2=[N:39]1

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 2724141Tetrabutylammonium FluorideHCID 667477259-(4-((Tert-butyl(dimethyl)silyl)oxy)phenyl)-3,4-dihydropyrido[2,1-c][1,2,4]thiadiazine 2,2-dioxide

生成物 1

HCID 667478174-(2,2-Dioxido-3,4-dihydropyrido[2,1-c][1,2,4]thiadiazin-9-yl)phenol収率 96.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

TBAF (1 M in THF) (40.0 mL) was added to a solution of 9-(4-{[tert-butyl(dimethyl)silyl]oxy}phenyl)-3,4-dihydropyrido[2,1-c][1,2,4]thiadiazine 2,2-dioxide (14.9 g) in THF (dry)(2.0 L) at 0° C. and the mixture was stirred at ambient temperature for 30 min. The mixture was neutralized with sat. NH4Cl aq. and extracted with EtOAc. The organic layer was separated, dried over anhydrous sodium sulfate and concentrated in vacuo. The residue was washed with EtOAc/hexane to give the title compound (10.2 g) as an off-white crystal.

後処理

  1. extractionextracted with EtOAc
  2. customThe organic layer was separated
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated in vacuo
  5. washThe residue was washed with EtOAc/hexane

出典と根拠

ORDレコード
ord-d8080b96cc5145bfb0d656910390739b
出典データセット
uspto-grants-2014_07
特許番号
US08778934B2

関連ノート

読み込み中…