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

HRID 1052446
ノート
印刷プレビュー

反応式

HRID 1052446 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6641367cbac34ae9879722a990b96bad
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09388189B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート