Ammonia → 4-Amino-6-chloro-N-(3-methoxy-4-(oxazol-5-yl)phenyl)pyrimidine-5-carboxamide

HRID 1052455노트

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HRID 1052455 반응식
[Cl:1][C:2]1[C:7]([C:8]([NH:10][C:11]2[CH:16]=[CH:15][C:14]([C:17]3[O:21][CH:20]=[N:19][CH:18]=3)=[C:13]([O:22][CH3:23])[CH:12]=2)=[O:9])=[C:6](Cl)[N:5]=[CH:4][N:3]=1.[NH3:25]>O1CCOCC1>[NH2:25][C:6]1[C:7]([C:8]([NH:10][C:11]2[CH:16]=[CH:15][C:14]([C:17]3[O:21][CH:20]=[N:19][CH:18]=3)=[C:13]([O:22][CH3:23])[CH:12]=2)=[O:9])=[C:2]([Cl:1])[N:3]=[CH:4][N:5]=1

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 901022024,6-Dichloro-N-(3-methoxy-4-(oxazol-5-yl)phenyl)pyrimidine-5-carboxamide

생성물 1

HCID 901032614-Amino-6-chloro-N-(3-methoxy-4-(oxazol-5-yl)phenyl)pyrimidine-5-carboxamide수율 98%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
0 °C

실험 절차

4,6-Dichloro-N-(3-methoxy-4-(oxazol-5-yl)phenyl)pyrimidine-5-carboxamide (844 mg, 2.01 mmol) was dissolved in dioxane (10 ml) and cooled in an ice bath. Ammonia solution (1.44 ml, 7N in MeOH) was added dropwise and the mixture was stirred at 0° C. for 20 min and 4 h at room temperature. After dilution with ethyl acetate, this organic phase was successively washed with water and brine, dried over magnesium sulphate, filtered and the solvents evaporated under reduced pressure, to yield a solid as a residue (788 mg, 86% purity, 98% yield) which was used in the next synthetic step without further purification.

후처리

  1. temperaturecooled in an ice bath
  2. washAfter dilution with ethyl acetate, this organic phase was successively washed with water and brine
  3. dry with materialdried over magnesium sulphate
  4. filtrationfiltered
  5. customthe solvents evaporated under reduced pressure
  6. customto yield a solid as a residue (788 mg, 86% purity, 98% yield) which
  7. customwas used in the next synthetic step without further purification

출처 및 근거

ORD 기록
ord-30e9697d4c374deebf441bf5f643f67c
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09388189B2

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