Potassium Hydroxide → 6-Fluoro-2(3H)-benzothiazolon-5-ylhydrazine

HRID 1709030

반응식

HRID 1709030 반응식
[NH2:1][C:2]1[C:3]([F:12])=[CH:4][C:5]2[S:9][C:8](=[O:10])[NH:7][C:6]=2[CH:11]=1.[N:13]([O-])=O.[Na+].[OH-].[K+]>Cl>[F:12][C:3]1[C:2]([NH:1][NH2:13])=[CH:11][C:6]2[NH:7][C:8](=[O:10])[S:9][C:5]=2[CH:4]=1

참가 물질

5

반응물 3

HCID 14797Potassium HydroxideHCID 144586855-amino-6-fluorobenzo[d]thiazol-2(3H)-oneHCID 23668193Sodium Nitrite

생성물 1

HCID 147716386-Fluoro-2(3H)-benzothiazolon-5-ylhydrazine수율 47%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매2회

실험 절차

A suspension of 5-amino-6-fluoro-2(3H)-benzothiazolone (12.98 g) in conc. hydrochloric acid (70 g) was cooled to 0° to 5° C., and a saturated aqueous solution of sodium nitrite (5.08 g) was dropwise added thereto at 0° to 5° C., followed by stirring at the same temperature for 30 minutes. The resultant mixture was cooled to -20° C., and a solution of stannous chloride (28.06 g) in conc. hydrochloric acid (30 g) was added thereto all at once, followed by stirring at 0° C. for 2 hours. The reaction mixture was neutralized with potassium hydroxide, a colloidal substance originated from stannous chloride was removed by celite and the resultant solution was extracted with ethyl acetate. The extract was washed with water, dried over magnesium sulfate and concentrated to give 6-fluoro-2(3H)-benzothiazolon-5-ylhydrazine (6.60 g).

후처리

  1. temperaturewas cooled to 0° to 5° C.
  2. customat 0° to 5° C.
  3. stirringby stirring at 0° C. for 2 hours
  4. customwas removed by celite
  5. extractionthe resultant solution was extracted with ethyl acetate
  6. washThe extract was washed with water
  7. dry with materialdried over magnesium sulfate
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-72adc180d26f4e7e89bcc32513f87f8e
출처 데이터셋
uspto-grants-1990_08
특허 번호
US04946961

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