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Hydrochloric Acid → HCID 14052568、化合物

HRID 330076
ノート
印刷プレビュー

反応式

HRID 330076 の反応式
Br[C:2]1[C:3]([F:11])=[C:4]([CH3:10])[C:5]([F:9])=[C:6]([F:8])[CH:7]=1.Cl.[CH3:13][N:14]1CCCC1=O>O>[F:11][C:3]1[C:4]([CH3:10])=[C:5]([F:9])[C:6]([F:8])=[CH:7][C:2]=1[C:13]#[N:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 13387N-methyl-2-pyrrolidoneHCID 140525671-Bromo-2,4,5-trifluoro-3-methylbenzene

生成物 1

HCID 14052568HCID 14052568、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 3-bromo-2,5,6-trifluorotoluene (11.0 g) and cupric cyanide (5.3 g) in N-methylpyrrolidone (15 ml) was stirred at 150° to 160° C. in a sealed tube for 4.5 hours. After cooling, to the reacting mixture was added a solution of ferric chloride (20 g) and concentrated hydrochloric acid (5 ml) in water (30 ml) and stirred at 50° to 60° C. for 20 minutes. The reacting mixture was extracted with ether, the organic layer was washed with aqueous hydrochloric acid solution, water and saturated aqueous sodium chloride solution successively, dried over anhydrous sodium sulfate and concentrated under reduced pressure to give the title compound (7.83 g) as pale brown oil.

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

後処理

  1. temperatureAfter cooling, to the reacting mixture
  2. stirringstirred at 50° to 60° C. for 20 minutes
  3. extractionThe reacting mixture was extracted with ether
  4. washthe organic layer was washed with aqueous hydrochloric acid solution, water and saturated aqueous sodium chloride solution successively
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-3400fbc7f7404634af49de6bfc2a5e4a
出典データセット
uspto-grants-1990_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04894458

反応ノート

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