HCID 11845249, 화합물 → 6,7-dihydro-4H-pyrazolo[5,1-c][1,4]thiazine-2-carbaldehyde

HRID 1158871노트

반응식

HRID 1158871 반응식
[N:1]1[N:9]2[C:4]([CH2:5][S:6][CH2:7][CH2:8]2)=[CH:3][C:2]=1[CH2:10][OH:11]>O=[Mn]=O.C(Cl)(Cl)Cl>[N:1]1[N:9]2[C:4]([CH2:5][S:6][CH2:7][CH2:8]2)=[CH:3][C:2]=1[CH:10]=[O:11]

참가 물질

4

반응물 1

HCID 11845249HCID 11845249, 화합물

생성물 1

HCID 118471336,7-dihydro-4H-pyrazolo[5,1-c][1,4]thiazine-2-carbaldehyde

시약·촉매·용매 2

HCID 14801Manganese dioxide촉매HCID 6212Chloroform용매

실험 절차

MnO2 (activated) (11.46 g) was added to the CHCl3 (135 mL) solution of (6,7-dihydro-4H-pyrazolo[5,1-c][1,4]thiazin-2-yl)methanol (2.31 g) and refluxed for 1 h under a nitrogen atmosphere. The reaction mixture was filtered through a pad of Celite. The filtrate was concentrated under a reduced pressure. The residue was applied to silica gel column chromatography, then the column was eluted with n-hexane—AcOEt (1/1). The titled compound was obtained as pale yellow crystals (1.78 g, 78%).

후처리

  1. temperaturerefluxed for 1 h under a nitrogen atmosphere
  2. filtrationThe reaction mixture was filtered through a pad of Celite
  3. concentrationThe filtrate was concentrated under a reduced pressure
  4. washthe column was eluted with n-hexane—AcOEt (1/1)

출처 및 근거

ORD 기록
ord-7ec9bc36c1f54989938c330e611c40b8
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07812014B2

반응 노트

불러오는 중…