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Water → 2-(2,6-Dichloro-4-trifluoromethylphenylhydrazino)succinonitrile

HRID 10767
ノート
印刷プレビュー

反応式

HRID 10767 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[C:4]([Cl:12])[C:3]=1[NH:13][N:14]=[C:15]([CH2:18][C:19]#[N:20])[C:16]#[N:17].[C-]#N.[Na+].O.C(=O)(O)[O-].[Na+]>C(O)(=O)C>[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([F:10])([F:11])[F:9])[CH:5]=[C:4]([Cl:12])[C:3]=1[NH:13][NH:14][CH:15]([CH2:18][C:19]#[N:20])[C:16]#[N:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8929Sodium CyanideHCID 516892Sodium BicarbonateHCID 853091952-(2,6-Dichloro-4-trifluoromethylphenylhydrazono)succinonitrile

生成物 1

HCID 539339412-(2,6-Dichloro-4-trifluoromethylphenylhydrazino)succinonitrile収率 40%

試薬・触媒・溶媒 1

HCID 176
Acetic Acid
溶媒

実験手順

2-(2,6-Dichloro-4-trifluoromethylphenylhydrazono) succinonitrile (0.296 g, 1 mmol), sodium cyanide (0.196 g, 4 equivalents), water (1 ml) and acetic acid (5 ml) were added successively to a tube, which was sealed and reacted at 20° C. for 40 hours. The mixture was added to saturated sodium bicarbonate solution, extracted (dichloromethane), washed (water), dried (magnesium sulfate) and evaporated to give a mixture which contained 40% of the desired title compound, NMR 3.1 (m, 2H), 4.5 (m, 1H), 5.89 (m, 1H), 6.94 (d, 1H), 7.71 (s, 2H), together with 60% of unchanged starting hydrazone.

後処理

  1. customwhich was sealed
  2. customreacted at 20° C. for 40 hours
  3. extractionextracted (dichloromethane)
  4. washwashed (water)
  5. dry with materialdried (magnesium sulfate)
  6. customevaporated
  7. customto give a mixture which

出典と根拠

ORDレコード
ord-baf1448600b24f08910c52ab2c44d07b
出典データセット
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07094906B2

反応ノート

読み込み中…

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