2-Hydrazinyl-N,N-dimethylethanamine → HCID 178427631, 화합물

HRID 234826

반응식

HRID 234826 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]([O-:24])[CH:17]=C[C:15]=3[C:14](=[O:25])[C:13]=2[C:12]([O:26][S:27]([C:30]2[CH:35]=[CH:34][C:33]([CH3:36])=[CH:32][CH:31]=2)(=[O:29])=[O:28])=[CH:11][CH:10]=1>C1COCC1.O>[C:33]1([CH3:36])[CH:32]=[CH:31][C:30]([S:27]([O:26][C:12]2[CH:11]=[CH:10][C:9]3[NH:6][N:5]=[C:4]4[C:3]5[CH:17]=[N+:18]([O-:24])[CH:19]=[CH:20][C:15]=5[C:14](=[O:25])[C:13]=2[C:22]=34)(=[O:28])=[O:29])=[CH:35][CH:34]=1

참가 물질

5

반응물 2

HCID 1205522-Hydrazinyl-N,N-dimethylethanamineHCID 233555479-Fluoro-6-(p-toluenesulfonyloxy)benzo[g]isoquinoline-5,10-dione-2-oxide

생성물 1

HCID 178427631HCID 178427631, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
40 °C

실험 절차

Under a nitrogen atmosphere a solution of N-[2-(dimethylamino)ethyl]hydrazine (0.805 g) in THF (10.75 mL) is added to a stirred suspension of 9-fluoro-6-(p-toluenesulfonyloxy)benzo[g]isoquinoline-5,10-dione-2-oxide of Preparative Example 21 (1.075 g) in THF (10.75 mL). After stirring for 2 h, the mixture is heated to 40° C. for 1 h. After cooling to room temperature the mixture is poured in water (150 mL) and the obtained suspension is stirred for 2 h. The precipitate is recovered by filtration and recrystallized from ethyl acetate/n-hexane to give 2-[2-(dimethylamino)ethyl)]-5-(p-toluenesulfonyloxy)isoquino[8,7,6-cd]indazole-6(2H)-one-9-oxide (0.31 g).

후처리

  1. temperatureAfter cooling to room temperature the mixture
  2. stirringthe obtained suspension is stirred for 2 h
  3. filtrationThe precipitate is recovered by filtration
  4. customrecrystallized from ethyl acetate/n-hexane

출처 및 근거

ORD 기록
ord-c45372fa41574a299e42b89c648ae329
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05596097

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