Water → 2-(3-(4-(2-pyrimidinyl)-1-piperazinyl)propyl)-7-methoxy-1,2,4-benzothiadiazin-3(4H)one 1,1dioxide

HRID 704883ノート

反応式

HRID 704883 の反応式
Br[CH2:2][CH2:3][CH2:4][N:5]1[C:10](=[O:11])[NH:9][C:8]2[CH:12]=[CH:13][C:14]([O:16][CH3:17])=[CH:15][C:7]=2[S:6]1(=[O:19])=[O:18].[N:20]1[CH:25]=[CH:24][CH:23]=[N:22][C:21]=1[N:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1.C(N(CC)CC)C.O>CN(C=O)C>[N:20]1[CH:25]=[CH:24][CH:23]=[N:22][C:21]=1[N:26]1[CH2:31][CH2:30][N:29]([CH2:2][CH2:3][CH2:4][N:5]2[C:10](=[O:11])[NH:9][C:8]3[CH:12]=[CH:13][C:14]([O:16][CH3:17])=[CH:15][C:7]=3[S:6]2(=[O:19])=[O:18])[CH2:28][CH2:27]1

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 887471-(2-Pyrimidinyl)piperazineHCID 190234312-(3-bromopropyl)-7-methoxy-1,2,4-benzothiadiazin-3(4H)one 1,1-dioxide

生成物 1

HCID 190234012-(3-(4-(2-pyrimidinyl)-1-piperazinyl)propyl)-7-methoxy-1,2,4-benzothiadiazin-3(4H)one 1,1dioxide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

0.01 mol of 2-(3-bromopropyl)-7-methoxy-1,2,4benzothiadiazin-3(4H)one 1,1-dioxide, 0.012 mol of 1-(2pyrimidinyl)piperazine and 0.01 mol of triethylamine are dissolved in 30 ml of DMF and the solution is heated at 60° C., with stirring, for 1.5 hours. Then 15 ml of water are added and the reaction mixture is cooled to 0° C. The substance which crystallises out during this is filtered off with suction, stirred with isopropanol, again filtered off with suction and dried in vacuo.

後処理

  1. temperaturethe reaction mixture is cooled to 0° C
  2. customThe substance which crystallises out during
  3. filtrationthis is filtered off with suction
  4. stirringstirred with isopropanol
  5. filtrationagain filtered off with suction
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-1e8f8854e5ca461aa6b15ee81b8ca2df
出典データセット
uspto-grants-1991_01
特許番号
US04988809

反応ノート

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