Diisopropylethylamine → HCID 178427630, 화합물

HRID 234823

반응식

HRID 234823 반응식
CN(C)[CH2:3][CH2:4][NH:5][NH2:6].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:6][N:5]=[C:4]4[C:3]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

참가 물질

7

반응물 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

생성물 1

HCID 178427630HCID 178427630, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매2회

실험 절차

Under a nitrogen atmosphere a solution of N-[2-(dimethylamino)ethyl]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 15b (2.4 g) in THF (24 mL) containing N,N-diisopropylethylamine (1.10 mL). A slightly exothermic reaction ensures, 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).

후처리

  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.

출처 및 근거

ORD 기록
ord-c208dc3912714dc6b557388c72cdbcae
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05596097

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