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HCID 178506935、化合物 → Bis(trifluoromethane)sulfonimide

HRID 1603251
ノート
印刷プレビュー

反応式

HRID 1603251 の反応式
[Li][N:2]([S:10]([C:13]([F:16])([F:15])[F:14])(=[O:12])=[O:11])[S:3]([C:6]([F:9])([F:8])[F:7])(=[O:5])=[O:4]>S(=O)(=O)(O)O>[NH:2]([S:3]([C:6]([F:9])([F:7])[F:8])(=[O:5])=[O:4])[S:10]([C:13]([F:16])([F:15])[F:14])(=[O:12])=[O:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 178506935HCID 178506935、化合物

生成物 1

HCID 157857Bis(trifluoromethane)sulfonimide収率 75.2%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

The imide HN(SO2CF3), was obtained from the lithium salt. LiN(SO2CF3)2 (10 g, 35 mmole) was added to 50 mL concentrated sulfuric acid. The free imide was distilled at about 90° C., 10 mm Hg and purified by sublimation at about 70° C., 1-2 mm Hg giving 7.4 g (74%) HN(SO2CF3)2. The silver salt was then obtained from the imide. Ag2CO3 (2.0 g, 0.2 mmol) was added slowly to a stirring, solution of HN(SO2CF3)2 (3.5 g, 12.0 mmole) in 25 mL water. The mixture was then digested, wrapped in foil, at 60° C. for 1 h and the excess Ag2CO3 filtered off. The water was removed under vacuum giving white powder of AgNTf2. Dissolution of the powder in diethyl ether (25 mL) followed by filtration and removal of all volatiles under vacuum gave 4.6 g (95%) of white AgNTf2.

後処理

  1. distillationThe free imide was distilled at about 90° C.
  2. custom10 mm Hg and purified by sublimation at about 70° C.

出典と根拠

ORDレコード
ord-2145ca0998694a1b9556477febad4fa7
出典データセット
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05986120

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート