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

HRID 428402노트

반응식

HRID 428402 반응식
[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

참가 물질

6

반응물 2

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

생성물 1

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

시약·촉매·용매 3

HCID 313Hydrochloric Acid촉매HCID 23925Iron촉매HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0e933289c5254e7881fbfb041a24797d
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06313295B1

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