HCID 59643067、化合物 → HCID 59643093、化合物

HRID 2251086ノート

反応式

HRID 2251086 の反応式
[CH3:1][N:2]1[C:6]([NH:7][C:8]2[C:13]([CH2:14][OH:15])=[CH:12][N:11]=[C:10]([S:16][CH3:17])[N:9]=2)=[CH:5][C:4]([CH3:18])=[N:3]1>C(Cl)Cl.C1COCC1.[O-2].[Mn+4].[O-2]>[CH3:1][N:2]1[C:6]([NH:7][C:8]2[C:13]([CH:14]=[O:15])=[CH:12][N:11]=[C:10]([S:16][CH3:17])[N:9]=2)=[CH:5][C:4]([CH3:18])=[N:3]1

参加物

4

反応物 1

HCID 59643067HCID 59643067、化合物

生成物 1

HCID 59643093HCID 59643093、化合物

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒HCID 21919333Tetrahydrofurane dichloromethane溶媒

実験手順

To a solution of [4-(2,5-dimethyl-2H-pyrazol-3-ylamino)-2-methylsulfanyl-pyrimidin-5-yl]-methanol, 17, (0.97 g, 3.66 mmol) in CH2Cl2/THF (35 mL of 1:1 mixture) is added manganese (IV) oxide (2.54 g, 29.28 mmol). After stirring the suspension at room temperature for 43 hours, the mixture is filtered through celite, and washed with CH2Cl2. The filtrate is concentrated in vacuo and the resulting residue is purified over silica (5% MeOH/chloroform) to afford 0.52 g of the desired product: 1H NMR (300 MHz, CDCl3) δ 8.22 (s, NH), 10.58 (s, NH), 9,86 (s, 1H), 8.54 (s, 1H), 6.36 (s, 1H), 3.81 (s, 3H), 2.58 (s, 3H), 2.30 (s, 3H); ESI+ MS: m/z (rel intensity) 264.0 (100, M++H).

後処理

  1. filtrationthe mixture is filtered through celite
  2. washwashed with CH2Cl2
  3. concentrationThe filtrate is concentrated in vacuo
  4. customthe resulting residue is purified over silica (5% MeOH/chloroform)

出典と根拠

ORDレコード
ord-cf54be082bec4752a60f77fcc1fa2f42
出典データセット
uspto-grants-2008_01
特許番号
US07319102B1

反応ノート

読み込み中…