Diisopropylethylamine → HCID 178427630、化合物

HRID 440360

反応式

HRID 440360 の反応式
CN([CH2:4][CH2:5][NH:6][NH2:7])C.F[C:9]1[C:22]2C(=O)[C:20]3[CH:19]=[N:18][CH:17]=C[C:15]=3[C:14](=[O:24])[C:13]=2[C:12]([O:25][S:26]([C:29]2[CH:34]=[CH:33][C:32]([CH3:35])=[CH:31][CH:30]=2)(=[O:28])=[O:27])=[CH:11][CH:10]=1.ClC1C2C(=O)C3C=NC=CC=3C(=O)C=2C(OS(C2C=CC(C)=CC=2)(=O)=O)=CC=1.C(N(CC)C(C)C)(C)C>C1COCC1.O>[C:32]1([CH3:35])[CH:31]=[CH:30][C:29]([S:26]([O:25][C:12]2[CH:11]=[CH:10][C:9]3[NH:7][N:6]=[C:5]4[C:4]5[CH:17]=[N:18][CH:19]=[CH:20][C:15]=5[C:14](=[O:24])[C:13]=2[C:22]=34)(=[O:28])=[O:27])=[CH:34][CH:33]=1

参加物

7

反応物 4

HCID 81531DiisopropylethylamineHCID 1205522-Hydrazinyl-N,N-dimethylethanamineHCID 105728809-Fluoro-6-(p-toluenesulfonyloxy)benzo[g]isoquinoline-5,10-dioneHCID 199747549-Chloro-6-(p-toluenesulfonyloxy)benzo[g]isoquinoline-5,10-dione

生成物 1

HCID 178427630HCID 178427630、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Under a nitrogen atmosphere a solution of 2-(dimethylaminoethyl)hydrazine (J. Med. Chem. 7, 493, 1964) (1.86 g) in anhydrous THF (6.0 mL) is added during 30' to the stirred 9:1 mixture of 9-fluoro-6-(p-toluenesulfonyloxy)benzo[g]isoquinoline-5,10-dione and 9-chloro-6-(p-toluenesulfonyloxy)benzo[g]isoquinoline-5,10-dione of Preparative Example 10b (2.4 g) in THF (24 mL) containing N,N-diisopropylethylamine (1.10 mL). A slightly exothermic reaction ensues, and the reaction temperature increases from 20° C. to 25° C. After one hour at room temperature the reaction mixture is poured in water (240 mL) and the suspension obtained is stirred for 30'. The solid is separated by suction, washed with water and dried at 40° C. to give 2-[2-(dimethylamino)ethyl)]-5-(p-toluenesulfonyloxy)isoquino[8,7,6-cd]indazole-6(2H)-one (1.44 g).

後処理

  1. customA slightly exothermic reaction
  2. temperaturethe reaction temperature increases from 20° C. to 25° C
  3. customthe suspension obtained
  4. stirringis stirred for 30'
  5. customThe solid is separated by suction
  6. washwashed with water
  7. customdried at 40° C.

出典と根拠

ORDレコード
ord-127deb16558d4906b4e0c73267926d33
出典データセット
uspto-grants-1996_05
特許番号
US05519029

関連ノート

読み込み中…