Isopropanol → (1-Methylethyl) [3-[[(4-methoxy-6-methylpyrimidin-2-yl)aminocarbonyl]aminosulfonyl]phenyl]carbamate

HRID 1262796

反応式

HRID 1262796 の反応式
[N:1]([C:4]1[CH:5]=[C:6]([S:10]([N:13]=[C:14]=[O:15])(=[O:12])=[O:11])[CH:7]=[CH:8][CH:9]=1)=[C:2]=[O:3].[NH2:16][C:17]1[N:22]=[C:21]([O:23][CH3:24])[CH:20]=[C:19]([CH3:25])[N:18]=1.[CH3:26][CH:27]([OH:29])[CH3:28]>C(Cl)Cl>[CH3:24][O:23][C:21]1[CH:20]=[C:19]([CH3:25])[N:18]=[C:17]([NH:16][C:14]([NH:13][S:10]([C:6]2[CH:5]=[C:4]([NH:1][C:2](=[O:3])[O:29][CH:27]([CH3:28])[CH3:26])[CH:9]=[CH:8][CH:7]=2)(=[O:11])=[O:12])=[O:15])[N:22]=1

参加物

5

反応物 3

HCID 3776IsopropanolHCID 5872364-Methoxy-6-methylpyrimidin-2-amineHCID 13138205m-Isocyanatobenzenesulfonyl isocyanate

生成物 1

HCID 13138206(1-Methylethyl) [3-[[(4-methoxy-6-methylpyrimidin-2-yl)aminocarbonyl]aminosulfonyl]phenyl]carbamate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To an anhydrous solution of 2.3 g of m-isocyanatobenzenesulfonyl isocyanate in 50 ml of methylene chloride was added in small portions 1.4 g of 2-amino-4-methoxy-6-methylpyrimidine. Efficient stirring was maintained during the addition and for three additional hours. The intermediate thus obtained, 3-isocyanto-N-[(4-methoxy-6-methylpyrimidin-2-yl)aminocarbonyl]benzenesulfonamide, was reacted further by adding one gram of 2 -propanol and stirring the resultant mixture for an additional sixteen hours. Filtration of the reaction mixture and evaporation of the filtrate yielded the desired product melting at 173°-180°.

後処理

  1. temperaturewas maintained during the addition and for three additional hours
  2. customThe intermediate thus obtained
  3. filtrationFiltration of the reaction mixture and evaporation of the filtrate

出典と根拠

ORDレコード
ord-9ece9c9fc41140b8b3a41f01c41e39a5
出典データセット
uspto-grants-1984_06
特許番号
US04453971

関連ノート

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