Water → 2-[2-[4-(2-Methoxyphenyl)-1-piperazinyl]ethyl]-6,7-dimethoxy-3,4-dihydro-1,2,4-benzothiadiazine-3-one 1,1-dioxide

HRID 986742ノート

反応式

HRID 986742 の反応式
[CH3:1][O:2][C:3]1[C:4]([O:16][CH3:17])=[CH:5][C:6]2[S:11](=[O:13])(=[O:12])[NH:10][C:9](=[O:14])[NH:8][C:7]=2[CH:15]=1.[H-].[Na+].[CH3:20][O:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1[N:28]1[CH2:33][CH2:32][N:31]([CH2:34][CH2:35]Cl)[CH2:30][CH2:29]1.O>CN(C)C=O>[CH3:20][O:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1[N:28]1[CH2:29][CH2:30][N:31]([CH2:34][CH2:35][N:10]2[C:9](=[O:14])[NH:8][C:7]3[CH:15]=[C:3]([O:2][CH3:1])[C:4]([O:16][CH3:17])=[CH:5][C:6]=3[S:11]2(=[O:13])=[O:12])[CH2:32][CH2:33]1

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 5956731-(2-Chloroethyl)-4-(2-methoxyphenyl)piperazineHCID 136505606,7-dimethoxy-3,4-dihydro-2H-1lambda6,2,4-benzothiadiazine-1,1,3-trione

生成物 1

HCID 136505612-[2-[4-(2-Methoxyphenyl)-1-piperazinyl]ethyl]-6,7-dimethoxy-3,4-dihydro-1,2,4-benzothiadiazine-3-one 1,1-dioxide収率 36%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
80 °C

実験手順

One gram and a half of 6,7-dimethoxy-3,4-dihydro-1,2,4-benzothiadiazine-3-one 1,1-dioxide was dissolved in 10 ml of dimethylformamide. After adding 280 mg of sodium hydride in 50% oil, the mixture was heated to 80° C. Then, a solution of 1.5 g of 2-[4-(2-methoxyphenyl)-1-piperazinyl]ethyl chloride in 5 ml of dimethylformamide was added dropwise to the resultant reaction liquid. After the addition was finished, the stirring was continued for 5 hours while heating at 80° C. to react. The resultant reaction mixture was poured into water to precipitate crystals. The produced crystals were filtered off followed by recrystallizing from methanol to obtain 1.0 g of the titled compound (yield: 36%).

後処理

  1. customreaction liquid
  2. additionAfter the addition
  3. temperaturewhile heating at 80° C.
  4. customto react
  5. customThe resultant reaction mixture
  6. customto precipitate crystals
  7. filtrationThe produced crystals were filtered off
  8. customby recrystallizing from methanol

出典と根拠

ORDレコード
ord-7b775669e1914ccda2b9c42056784f01
出典データセット
uspto-grants-1987_12
特許番号
US04716161

反応ノート

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