1-(2-Hydrazinylethyl)pyrrolidine → 9-Methoxy-5-nitro-2-[2-(1-pyrrolidinyl)ethyl]-2H-[1]-benzopyrano[4,3,2-cd]indazole, monohydrochloride

HRID 364167

反応式

HRID 364167 の反応式
[Cl:1][C:2]1[C:15]2[C:14](=O)[C:13]3[C:8](=[CH:9][CH:10]=[C:11]([O:17][CH3:18])[CH:12]=3)[O:7][C:6]=2[C:5]([N+:19]([O-:21])=[O:20])=[CH:4][CH:3]=1.[NH:22]([CH2:24][CH2:25][N:26]1[CH2:30][CH2:29][CH2:28][CH2:27]1)[NH2:23]>C1COCC1>[ClH:1].[CH3:18][O:17][C:11]1[CH:10]=[CH:9][C:8]2[O:7][C:6]3[C:15]4[C:14](=[N:23][N:22]([CH2:24][CH2:25][N:26]5[CH2:30][CH2:29][CH2:28][CH2:27]5)[C:2]=4[CH:3]=[CH:4][C:5]=3[N+:19]([O-:21])=[O:20])[C:13]=2[CH:12]=1

参加物

4

反応物 2

HCID 30315561-(2-Hydrazinylethyl)pyrrolidineHCID 136890881-Chloro-7-methoxy-4-nitro-9H-xanthen-9-one

生成物 1

HCID 1317148059-Methoxy-5-nitro-2-[2-(1-pyrrolidinyl)ethyl]-2H-[1]-benzopyrano[4,3,2-cd]indazole, monohydrochloride

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 12.2 g of 1-chloro-7-methoxy-4-nitro-9H-xanthen-9-one and 11.0 g of 1-(2-hydrazinoethyl)pyrrolidine in 200 ml of THF was stirred 20 hours at room temperature. The orange liquor was decanted, freed of solvent under reduced pressure, and the residue, in chloroform, was chromatographed over silica gel, eluting with chloroform-methanol (25:1 by volume). The desired fractions yielded the free base of the title compound, mp 140°-142° C.

後処理

  1. customThe orange liquor was decanted
  2. customthe residue, in chloroform, was chromatographed over silica gel
  3. washeluting with chloroform-methanol (25:1 by volume)

出典と根拠

ORDレコード
ord-89315955443e42b683b57d0ac48944ff
出典データセット
uspto-grants-1986_08
特許番号
US04604390

関連ノート

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