반응 #3354

반응 방정식

NaOH

2,2'-Dithiobis(5-nitrobenzamide)

acetic acid

→

2,2'-Dithiobis(5-aminobenzamide)

용매

water

반응 조건

후처리

1. 1
   온도The resulting slurry was heated
2. 2
   온도at reflux for 2.0 hours
3. 3
   여과The alkaline mixture was filtered
4. 4
   workup.ADDITIONacetic acid was added to the solution
5. 5
   기타While bubbling oxygen into the solution
6. 6
   온도a pH=6-7 was maintained with the addition of acetic acid
7. 7
   기타A solid gradually formed as the pH
8. 8
   여과The product (1.1 g) was recovered by filtration, mp 188°-190° C.

실험 절차

2,2'-Dithiobis(5-nitrobenzamide) (2.6 g, 7.0 mmol) was added portion-wise to a refluxing slurry of reduced iron (8.7 g) in 65 mL of water containing 0.1 mL of acetic acid. The resulting slurry was heated at reflux for 2.0 hours, then cooled to room temperature. The slurry was made strongly basic (pH 11) by the addition of 14 mL of 1N NaOH. The alkaline mixture was filtered, and acetic acid was added to the solution to adjust the pH to 7.0. While bubbling oxygen into the solution, a pH=6-7 was maintained with the addition of acetic acid. A solid gradually formed as the pH begins to stabilize. The product (1.1 g) was recovered by filtration, mp 188°-190° C.

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