Nitric Acid → 6-fluoro-5-nitro-2(3H)-benzothiazolone

HRID 1199147

반응식

HRID 1199147 반응식
[F:1][C:2]1[CH:11]=[CH:10][C:5]2[NH:6][C:7](=[O:9])[S:8][C:4]=2[CH:3]=1.[N+:12]([O-])([OH:14])=[O:13]>S(=O)(=O)(O)O>[F:1][C:2]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][C:5]2[NH:6][C:7](=[O:9])[S:8][C:4]=2[CH:3]=1

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 446672-Benzothiazolinone, 6-fluoro-

생성물 1

HCID 139579556-fluoro-5-nitro-2(3H)-benzothiazolone수율 80.5%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

A solution of 6-fluoro-2(3H)-benzothiazolone (47.58 g) in 100% sulfuric acid (760 ml) was cooled at 0° to 5° C., and 98% fuming nitric acid (d=1.52; 18.79 g) was dropwise added thereto, followed by stirring at the same temperature for 60 minutes. The reaction mixture was poured into ice-water. The precipitated crystals were collected by filtration, washed with water and dried to give 6-fluoro-5-nitro-2(3H)-benzothiazolone (48.48 g) as pale brown crystals. m.p., 180°-182° C.

후처리

  1. filtrationThe precipitated crystals were collected by filtration
  2. washwashed with water
  3. customdried

출처 및 근거

ORD 기록
ord-258ce2a18b5a4c14b959a911fcca3b07
출처 데이터셋
uspto-grants-1990_02
특허 번호
US04898948

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