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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Methanol → 2,8-dibromo-5,5-dioxo-5H-5lambda6-dibenzothiophene-3,7-diamine

HRID 376732
ノート
印刷プレビュー

反応式

HRID 376732 の反応式
[Br:1][C:2]1[C:20]([N+:21]([O-])=O)=[CH:19][C:5]2[S:6](=[O:18])(=[O:17])[C:7]3[CH:12]=[C:11]([N+:13]([O-])=O)[C:10]([Br:16])=[CH:9][C:8]=3[C:4]=2[CH:3]=1.[Sn](Cl)Cl.[H][H].CO>[Pd].[Fe].[Zn].C(O)(=O)C.COCCO.C(O)CC.C(O)C>[Br:1][C:2]1[C:20]([NH2:21])=[CH:19][C:5]2[S:6](=[O:18])(=[O:17])[C:7]3[CH:12]=[C:11]([NH2:13])[C:10]([Br:16])=[CH:9][C:8]=3[C:4]=2[CH:3]=1
参加物実験手順出典と根拠反応ノート

参加物

12

反応物 4

HCID 887MethanolHCID 24479Stannous ChlorideHCID 4571975Dibenzothiophene, 2,8-dibromo-3,7-dinitro-, 5,5-dioxideHCID 178418361HCID 178418361、化合物

生成物 1

HCID 158859562,8-dibromo-5,5-dioxo-5H-5lambda6-dibenzothiophene-3,7-diamine

試薬・触媒・溶媒 7

HCID 23925Iron
触媒
HCID 23938Palladium触媒
HCID 23994Zinc触媒
HCID 176Acetic Acid溶媒
HCID 702Ethanol溶媒
HCID 10311-Propanol溶媒
HCID 80192-Methoxyethanol溶媒

実験手順

Referring to Scheme II, a mixture of 2,8-dibromo-3,7-dinitrodibenzothiophene-5-oxide 3a and 2,8-dibromo-3-nitrodibenzothiophene-5-oxide 3b was treated in a heterogeneous solvent mixture which include but not limited to acetonitrile, carbon tetrachloride and water, p-dioxane and water, acetonitrile, tetrahydrofuran and water; with an oxidizing agent which include but not limited to sodium periodate and ruthenium(III) chloride; stirred at a temperature range from 15-75° C. until completion as indicated by TLC to yield 2,8-dibromo-3,7-dinitrodibenzothiophene-5,5-dioxide 9 as the isolated product. Treating 2,8-dibromo-3,7-dinitrodibenzothiophen-5,5-dioxide 9 with a reducing agent which include but are not limited to powdered iron, tin (II) chloride, zinc metal or palladium on charcoal with hydrogen in alcoholic solvents which include but are not limited to methyl alcohol, ethyl alcohol, propyl alcohol or 2-methoxy-ethanol and the like; and an organic acid which includes but is not limited to acetic acid; at a temperature range from 50-120° C. for about 2 hours or until completion to give 2,8-dibromo-5,5-dioxo-5H-5λ6 -dibenzothiophene-3,7-diamine 10.

出典と根拠

ORDレコード
ord-7a672bb9033e49159e7c343b3b16934d
出典データセット
uspto-grants-2000_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06022307

反応ノート

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