HCID 59643067, 화합물 → HCID 59643093, 화합물

HRID 2251086노트

반응식

HRID 2251086 반응식
[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

참가 물질

4

반응물 1

HCID 59643067HCID 59643067, 화합물

생성물 1

HCID 59643093HCID 59643093, 화합물

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매HCID 21919333Tetrahydrofurane dichloromethane용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-cf54be082bec4752a60f77fcc1fa2f42
출처 데이터셋
uspto-grants-2008_01
특허 번호
US07319102B1

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