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Hydrochloric Acid → N-(4,4,4-trinitrobutyryl)-N'-(perfluorobutyryl)hydrazine

HRID 2255673
ノート
印刷プレビュー

反応式

HRID 2255673 の反応式
[N+:1]([C:4]([N+:13]([O-:15])=[O:14])([N+:10]([O-:12])=[O:11])[CH2:5][CH2:6][C:7](Cl)=[O:8])([O-:3])=[O:2].[F:16][C:17]([F:29])([C:25]([F:28])([F:27])[F:26])[C:18]([F:24])([F:23])[C:19]([NH:21][NH2:22])=[O:20].N1C=CC=CC=1.Cl>C(OCC)C.O>[N+:1]([C:4]([N+:13]([O-:15])=[O:14])([N+:10]([O-:12])=[O:11])[CH2:5][CH2:6][C:7]([NH:22][NH:21][C:19](=[O:20])[C:18]([F:23])([F:24])[C:17]([F:16])([F:29])[C:25]([F:27])([F:26])[F:28])=[O:8])([O-:3])=[O:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 2467902,2,3,3,4,4,4-HeptafluorobutanehydrazideHCID 125075564,4,4-Trinitrobutyryl chloride

生成物 1

HCID 19738486N-(4,4,4-trinitrobutyryl)-N'-(perfluorobutyryl)hydrazine

試薬・触媒・溶媒 2

HCID 962Water
溶媒
HCID 3283Diethyl Ether溶媒2 回

実験手順

To a solution of 1.0 g (0.0041 mole) of 4,4,4-trinitrobutyryl chloride in anhydrous diethyl ether (10 mL) stirred at 20° C. (water bath) was added 0.9 g (0.0039 mole) of N-(heptafluorobutyryl)hydrazine. The mixture became thick with precipitate and sufficient ether (10 mL) was added to allow efficient stirring. Pyridine (0.35 ml, 0.0044 mole) was added dropwise and the mixture was stirred for 5 minutes before 5% hydrochloric acid (10 mL) was added. The ether layer was dried (Na2SO4), the volatiles were removed, and the residue was stirred with water to give 1.5 g, mp 146°-150° C. Crystallization from 1,2-dichloroethane gave the product, N-(4,4,4-trinitrobutyryl)-N'-(perfluorobutyryl)hydrazine, 1.2 g (70%) mp 154°-156° C.; 1H NMR (acetone-d6 +D2O): 2.98 (t, 2H), 3.87 (t, 2H).

後処理

  1. additionwas added
  2. additionwas added
  3. dry with materialThe ether layer was dried (Na2SO4)
  4. customthe volatiles were removed
  5. customto give 1.5 g, mp 146°-150° C
  6. customCrystallization from 1,2-dichloroethane

出典と根拠

ORDレコード
ord-5713548f3a114501a9236327274a1db9
出典データセット
uspto-grants-1993_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05241071

反応ノート

読み込み中…

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