Stannous Chloride → 3-Chloro-5-hydrazino-phenol

HRID 1517648

反応式

HRID 1517648 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([OH:9])[CH:5]=[C:6]([Cl:8])[CH:7]=1.[N:10]([O-])=O.[Na+].[Sn](Cl)Cl.C(=O)([O-])O.[Na+]>Cl.O>[Cl:8][C:6]1[CH:5]=[C:4]([OH:9])[CH:3]=[C:2]([NH:1][NH2:10])[CH:7]=1

参加物

7

反応物 4

HCID 24479Stannous ChlorideHCID 516892Sodium BicarbonateHCID 199869473-Amino-5-chlorophenolHCID 23668193Sodium Nitrite

生成物 1

HCID 552816153-Chloro-5-hydrazino-phenol

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒2 回HCID 962Water溶媒2 回

反応条件

温度
0 °C

実験手順

2.1 g (14.3 mmol) 3-amino-5-chloro-phenol are dissolved in 20 ml of conc. hydrochloric acid and 20 ml of water and cooled to 0° C. 1.0 g (15.0 mmol) sodium nitrite in 4 ml of water are added. Then a solution of 12.1 g (53.5 mmol) tin(II)-chloride in 16 ml hydrochloric acid is slowly added dropwise at −5° C. It is stirred for 1 hour at 0° C., then adjusted to pH7 with sodium hydrogen carbonate. The precipitate formed is suction filtered and washed with water. The filtrate is extracted with diethyl ether. The organic phase is dried and evaporated to dryness. The residue is extracted with hexane.

後処理

  1. customThe precipitate formed
  2. filtrationfiltered
  3. washwashed with water
  4. extractionThe filtrate is extracted with diethyl ether
  5. customThe organic phase is dried
  6. customevaporated to dryness
  7. extractionThe residue is extracted with hexane

出典と根拠

ORDレコード
ord-f51cbabc9ec145f4b2067317581ab2c5
出典データセット
uspto-grants-2012_07
特許番号
US08232286B2

関連ノート

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