2,4-Dichloro-6-fluoro-7-nitrobenzothiazole → 7-Amino-2,4-dichloro-6-fluorobenzothiazole

HRID 21725노트

반응식

HRID 21725 반응식
[Cl:1][C:2]1[S:3][C:4]2[C:10]([N+:11]([O-])=O)=[C:9]([F:14])[CH:8]=[C:7]([Cl:15])[C:5]=2[N:6]=1>C(O)(=O)C.C(OCC)(=O)C.[Fe]>[NH2:11][C:10]1[C:4]2[S:3][C:2]([Cl:1])=[N:6][C:5]=2[C:7]([Cl:15])=[CH:8][C:9]=1[F:14]

참가 물질

5

반응물 1

HCID 199334652,4-Dichloro-6-fluoro-7-nitrobenzothiazole

생성물 1

HCID 199334577-Amino-2,4-dichloro-6-fluorobenzothiazole

시약·촉매·용매 3

HCID 23925Iron촉매HCID 176Acetic Acid용매2회HCID 8857Ethyl Acetate용매

실험 절차

5 g Iron powder was added to 40 ml 5% aqueous acetic acid. The mixture was heated to reflux and a solution of 5 g 2,4-dichloro-6-fluoro-7-nitrobenzothiazole in 40 ml acetic acid and 40 ml ethyl acetate was added. The mixture was heated for 2 hours under reflux and after cooling the mixture was filtered over celite, the phases separated and the aqueous phase extracted with ethyl acetate. The combined organic phases were washed with aqueous sodium hydrogen carbonate and water and dried with magnesium sulfate. Yield: 4.3 g=97% of theory m.p.: 173° C.

후처리

  1. temperatureThe mixture was heated
  2. temperatureto reflux
  3. temperatureThe mixture was heated for 2 hours
  4. temperatureunder reflux
  5. temperatureafter cooling the mixture
  6. filtrationwas filtered over celite
  7. customthe phases separated
  8. extractionthe aqueous phase extracted with ethyl acetate
  9. washThe combined organic phases were washed with aqueous sodium hydrogen carbonate and water
  10. dry with materialdried with magnesium sulfate

출처 및 근거

ORD 기록
ord-85822b54c9224dcdb1b547c04bcbde94
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05424443

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