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

HRID 2235498ノート

反応式

HRID 2235498 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

HCID 43257247-Nitro-1,3-benzothiazol-2-amine収率 51.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 5943Carbon Tetrachloride溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-50d2f6438b6149d9a13e9cc78b5d1609
出典データセット
uspto-grants-2010_05
特許番号
US07714009B2

反応ノート

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