Potassium Carbonate → 7-Nitro-1,3-benzothiazol-2-amine

HRID 2235498노트

반응식

HRID 2235498 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([NH:10][C:11]([NH2:13])=[S:12])[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2].BrBr.C(=O)([O-])[O-].[K+].[K+]>C(Cl)(Cl)(Cl)Cl.O>[N+:1]([C:4]1[C:5]2[S:12][C:11]([NH2:13])=[N:10][C:6]=2[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 24408BromineHCID 2754758(3-Nitrophenyl)thiourea

생성물 1

HCID 43257247-Nitro-1,3-benzothiazol-2-amine수율 51.2%

시약·촉매·용매 2

HCID 962Water용매HCID 5943Carbon Tetrachloride용매2회

실험 절차

To 0.60 g (3.0 mmol) of (3-nitrophenyl)thiourea in 25 mL of carbon tetrachloride was added 0.17 mL (3.4 mmol) of bromine in 10 mL of carbon tetrachloride dropwise over 1 h. The mixture was heated to reflux for 18 h, cooled to room temperature and the precipitate that formed was collected by filtration. The precipitate was slurried in glacial acetic acid and the solids were collected by filtration. The solids thus obtained were slurried in water and saturated potassium carbonate was added until the pH was about 9. The free base was collected by filtration to give 0.30 g (51%) of the title compound as a light orange solid.

후처리

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 18 h
  3. customthe precipitate that formed
  4. filtrationwas collected by filtration
  5. filtrationthe solids were collected by filtration
  6. customThe solids thus obtained
  7. filtrationThe free base was collected by filtration

출처 및 근거

ORD 기록
ord-50d2f6438b6149d9a13e9cc78b5d1609
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07714009B2

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