Ammonia → HCID 90103324、化合物

HRID 1052641ノート

反応式

HRID 1052641 の反応式
[Cl:1][C:2]1[C:7]([C:8]([NH:10][C:11]2[CH:16]=[C:15]([NH:17][S:18]([CH3:21])(=[O:20])=[O:19])[CH:14]=[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]=[C:15]([NH:17][S:18]([CH3:21])(=[O:20])=[O:19])[CH:14]=[C:13]([O:22][CH3:23])[CH:12]=2)=[O:9])=[C:2]([Cl:1])[N:3]=[CH:4][N:5]=1

参加物

4

反応物 2

HCID 222AmmoniaHCID 901021774,6-Dichloro-N-(3-methoxy-5-(methylsulfonamido)phenyl)pyrimidine-5-carboxamide

生成物 1

HCID 90103324HCID 90103324、化合物収率 155.7%

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-methoxy-5-(methylsulfonamido)phenyl)pyrimidine-5-carboxamide (617 mg, 73% purity, 1.14 mmol) was dissolved in dioxane (5 ml) and cooled in an ice bath. Ammonia (819 μl, 7N in MeOH, 5.7 mmol) was added dropwise and the mixture stirred at 0° C. for 6 h and at room temperature overnight. The solvent was removed and ethyl acetate added. The solid precipitate was filtered off and the filtrate was concentrated to give 660 mg (100% yield) of the title compound as an oil that was used in the next step without further purification. Purity 65%

後処理

  1. temperaturecooled in an ice bath
  2. customThe solvent was removed
  3. additionethyl acetate added
  4. filtrationThe solid precipitate was filtered off
  5. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-e57255a6e0174b41a4ad203abf1734d1
出典データセット
uspto-grants-2016_07
特許番号
US09388189B2

反応ノート

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