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

HRID 1517648노트

반응식

HRID 1517648 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

HCID 552816153-Chloro-5-hydrazino-phenol

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매2회HCID 962Water용매2회

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f51cbabc9ec145f4b2067317581ab2c5
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08232286B2

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