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Ammonia → HCID 90102281, 화합물

HRID 1052461
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HRID 1052461 반응식
[Cl:1][C:2]1[C:7]([C:8]([NH:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[O:17][CH3:18])=[O:9])=[C:6](Cl)[N:5]=[CH:4][N:3]=1.[NH3:20]>O1CCOCC1>[NH2:20][C:6]1[C:7]([C:8]([NH:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[O:17][CH3:18])=[O:9])=[C:2]([Cl:1])[N:3]=[CH:4][N:5]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 901027264,6-Dichloro-N-(2-methoxyphenyl)-5-pyrimidinecarboxamide

생성물 1

HCID 90102281HCID 90102281, 화합물수율 95.8%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
0 °C

실험 절차

4,6-Dichloro-N-(2-methoxyphenyl)pyrimidine-5-carboxamide (506 mg, 1.70 mmol) was dissolved in dioxane (8 ml) and cooled in an ice bath. Ammonia solution (1.25 ml, 8.75 mmol, 7N in MeOH) was added dropwise and the mixture was stirred at 0° C. for 6 h. After evaporation of the solvent under reduced pressure, the residue was suspended in ethyl acetate and filtered, washing successively with ethyl acetate. The solvent of the filtrate is evaporated under reduced pressure to yield the final compound as a solid (454 mg, 93% purity, 89% yield) which was used in the next synthetic step without further purification.

후처리

  1. temperaturecooled in an ice bath
  2. customAfter evaporation of the solvent under reduced pressure
  3. filtrationfiltered
  4. washwashing successively with ethyl acetate
  5. customThe solvent of the filtrate is evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-bf189cd303504b40af94458340927287
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09388189B2

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