Water → 1,2-Benzisothiazol-5-amine, 3-chloro-

HRID 48980ノート

反応式

HRID 48980 の反応式
[Cl:1][C:2]1[C:6]2[CH:7]=[C:8]([N+:11]([O-])=O)[CH:9]=[CH:10][C:5]=2[S:4][N:3]=1.O>C1(C)C=CC=CC=1.Cl.[Fe]>[NH2:11][C:8]1[CH:9]=[CH:10][C:5]2[S:4][N:3]=[C:2]([Cl:1])[C:6]=2[CH:7]=1

参加物

6

反応物 2

HCID 962WaterHCID 1980981,2-Benzisothiazole, 3-chloro-5-nitro-

生成物 1

HCID 1987661,2-Benzisothiazol-5-amine, 3-chloro-

試薬・触媒・溶媒 3

HCID 313Hydrochloric Acid触媒HCID 23925Iron触媒HCID 1140Toluene溶媒

実験手順

A solution of 3-chloro-5-nitro-1,2-benzisothiazole (2.00 g) in toluene is treated with iron powder (8.40 g, 325 mesh) and concentrated hydrochloric acid (8 drops), heated to reflux, treated dropwise with water (8.00 mL), refluxed for 35 minutes, cooled to room temperature, and filtered through diatomaceous earth. The resultant filtrate is concentrated in vacuo to obtain a residue. Flash column chromatography of the residue using silica gel and an ethyl acetate/hexanes solution (1:1) gives the title product.

後処理

  1. temperatureheated
  2. temperatureto reflux
  3. temperaturerefluxed for 35 minutes
  4. filtrationfiltered through diatomaceous earth
  5. concentrationThe resultant filtrate is concentrated in vacuo
  6. customto obtain a residue

出典と根拠

ORDレコード
ord-2491bb556efb4af9bb365b55cb57ad4f
出典データセット
uspto-grants-2004_03
特許番号
US06706663B2

反応ノート

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