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

HRID 1747943

반응식

HRID 1747943 반응식
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

참가 물질

5

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f1dcb8d3bb2742659da939bc8c69b7dc
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09150591B2

연결된 노트

불러오는 중…