Ethyl Acetate → 7-Amino-4-chloro-6-fluoro-2-methylbenzothiazole

HRID 1419711노트

반응식

HRID 1419711 반응식
[Cl:1][C:2]1[C:7]2[N:8]=[C:9]([CH3:11])[S:10][C:6]=2[C:5]([N+:12]([O-])=O)=[C:4]([F:15])[CH:3]=1.C(OCC)(=O)C>O.Cl.[Fe]>[NH2:12][C:5]1[C:6]2[S:10][C:9]([CH3:11])=[N:8][C:7]=2[C:2]([Cl:1])=[CH:3][C:4]=1[F:15]

참가 물질

6

반응물 2

HCID 8857Ethyl AcetateHCID 537041054-Chloro-6-fluoro-2-methyl-7-nitrobenzothiazole

생성물 1

HCID 537099237-Amino-4-chloro-6-fluoro-2-methylbenzothiazole

시약·촉매·용매 3

HCID 23925Iron촉매HCID 313Hydrochloric Acid용매HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

6 g of iron powder were added to a suspension of 8 g (32 mmol) of 4-chloro-6-fluoro-2-methyl-7-nitrobenzothiazole in 100 ml of water and 9 ml of concentrated hydrochloric acid, which suspension had been heated to 80° C., after which the mixture was refluxed for 3 hours. 200 ml of ethyl acetate were then added to the reaction mixture. The solid was filtered off. The remaining organic phase was washed with water, dried over magnesium sulfate and finally evaporated down. Yield: 4.5 g.

후처리

  1. temperatureafter which the mixture was refluxed for 3 hours
  2. filtrationThe solid was filtered off
  3. washThe remaining organic phase was washed with water
  4. dry with materialdried over magnesium sulfate
  5. customfinally evaporated down

출처 및 근거

ORD 기록
ord-37de1006222e41ceac0e5112e086f55f
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05888940

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