Water → 5-Bromo-6-chloro-2-(1H-pyrazol-1-yl)-4-pyrimidinamine

HRID 2401163

반응식

HRID 2401163 반응식
[Br:1][C:2]1[C:3]([NH2:12])=[N:4][C:5](S(C)=O)=[N:6][C:7]=1[Cl:8].[NH:13]1[CH:17]=[CH:16][CH:15]=[N:14]1.C(=O)([O-])[O-].[Cs+].[Cs+].O>CN(C=O)C>[Br:1][C:2]1[C:3]([NH2:12])=[N:4][C:5]([N:13]2[CH:17]=[CH:16][CH:15]=[N:14]2)=[N:6][C:7]=1[Cl:8]

참가 물질

6

반응물 4

HCID 962WaterHCID 1048PyrazoleHCID 10796Cesium carbonateHCID 866770165-Bromo-6-chloro-2-methanesulfinylpyrimidin-4-amine2회

생성물 1

HCID 866770175-Bromo-6-chloro-2-(1H-pyrazol-1-yl)-4-pyrimidinamine수율 65%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1 g (3.7 mmol) of 5-bromo-6-chloro-2-(methylsulfinyl)pyrimidine-4-amine (intermediate 2) was suspended in 10 ml of DMF. To this suspension were added 0.33 g (4.8 mmol) de pyrazole and 0.8 g of cesium carbonate. The reaction mixture was turned immediately light yellow color and allowed to stir at room temperature for about 1 to 2 hours. After nearly complete conversion to the corresponding monosubstituted derivative as was indicated by TLC the solution was poured onto 100 ml of cool water. The formed precipitated was filtered, washed with water and dried to afford 0.66 g (65%) of the desired product.

후처리

  1. customThe formed precipitated
  2. filtrationwas filtered
  3. washwashed with water
  4. customdried

출처 및 근거

ORD 기록
ord-be51a176488d42638229ef21fd1ee146
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08796284B2

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