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Ammonia → 4-Amino-6-chloro-N-(3,5-dimethoxyphenyl)-5-pyrimidinecarboxamide

HRID 1052446
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HRID 1052446 반응식
[Cl:1][C:2]1[C:7]([C:8]([NH:10][C:11]2[CH:16]=[C:15]([O:17][CH3:18])[CH:14]=[C:13]([O:19][CH3:20])[CH:12]=2)=[O:9])=[C:6](Cl)[N:5]=[CH:4][N:3]=1.[NH3:22]>O1CCOCC1>[NH2:22][C:6]1[C:7]([C:8]([NH:10][C:11]2[CH:16]=[C:15]([O:17][CH3:18])[CH:14]=[C:13]([O:19][CH3:20])[CH:12]=2)=[O:9])=[C:2]([Cl:1])[N:3]=[CH:4][N:5]=1
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참가 물질

4

반응물 2

HCID 222AmmoniaHCID 901035974,6-Dichloro-N-(3,5-dimethoxyphenyl)-5-pyrimidinecarboxamide

생성물 1

HCID 901027364-Amino-6-chloro-N-(3,5-dimethoxyphenyl)-5-pyrimidinecarboxamide수율 100%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
0 °C

실험 절차

4,6-Dichloro-N-(3,5-dimethoxyphenyl)pyrimidine-5-carboxamide (684 mg, 1.21 mmol) was dissolved in dioxane (5 ml) and cooled in an ice bath. Ammonia solution (0.86 ml, 7N in MeOH) was added dropwise and the mixture was stirred at 0° C. for 6 h and overnight at room temperature. After dilution with ethyl acetate, this organic phase was washed with water and brine, dried over magnesium sulphate, filtered and the solvents evaporated under reduced pressure, to yield an oil as a residue (575 mg, 66% purity, 100% 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 washed with water and brine
  3. dry with materialdried over magnesium sulphate
  4. filtrationfiltered
  5. customthe solvents evaporated under reduced pressure
  6. customto yield an oil as a residue (575 mg, 66% purity, 100% yield) which
  7. customwas used in the next synthetic step without further purification

출처 및 근거

ORD 기록
ord-6641367cbac34ae9879722a990b96bad
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09388189B2

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