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

HRID 1158871ノート

反応式

HRID 1158871 の反応式
[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]

参加物

4

反応物 1

HCID 11845249HCID 11845249、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 14801Manganese dioxide触媒HCID 6212Chloroform溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-7ec9bc36c1f54989938c330e611c40b8
出典データセット
uspto-grants-2010_10
特許番号
US07812014B2

反応ノート

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