Hydrochloric Acid → 3-Chloropyridine-2-sulfonamide

HRID 1154533노트

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HRID 1154533 반응식
ClC1C(SCC2C=CC=CC=2)=[N:4]C=CC=1.ClCl.C([O-])(=O)C.[Na+].[Cl:23][C:24]1[C:25]([S:30](Cl)(=[O:32])=[O:31])=[N:26][CH:27]=[CH:28][CH:29]=1.Cl>O.C(O)(=O)C>[Cl:23][C:24]1[C:25]([S:30]([NH2:4])(=[O:32])=[O:31])=[N:26][CH:27]=[CH:28][CH:29]=1

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 24526ChlorineHCID 517045Sodium Acetate2회HCID 179110873-Chloropyridine-2-sulfonyl chloride2회HCID 19881832Pyridine, 3-chloro-2-[(phenylmethyl)thio]-

생성물 1

HCID 146531913-Chloropyridine-2-sulfonamide

시약·촉매·용매 2

HCID 176Acetic Acid용매2회HCID 962Water용매2회

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온도
-30 °C

실험 절차

53.0 Grams (0.225 mole) of 3-chloro-2-((phenylmethyl)thio)pyridine were added to 250 ml of acetic acid containing 16.2 grams (0.90 mole) of water. The mixture was cooled in an ice bath and passed in a stream of chlorine at 10°-15° C. for 31/2 hours. The resulting cold acetic acid solution was poured, with stirring, into a mixture of 180 grams (2.2 moles) of sodium acetate, 500 ml water and 250 grams crushed ice. (The sodium acetate converts the 3-chloro-2-pyridine sulfonyl chloride present as the hydrochloride, into free 3-chloro-2-pyridine sulfonyl chloride.) The resulting mixture was extracted with methylene chloride, washed with water, and dried over anhydrous sodium sulfate. The methylene chloride extract was evaporated to 150 ml and cooled to -30° C. in a dry ice bath.

후처리

  1. temperatureThe mixture was cooled in an ice bath
  2. custom2 hours
  3. customcrushed ice
  4. extraction) The resulting mixture was extracted with methylene chloride
  5. washwashed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. extractionThe methylene chloride extract
  8. customwas evaporated to 150 ml

출처 및 근거

ORD 기록
ord-f150ec48317d4586af92cc40b33e64e2
출처 데이터셋
uspto-grants-1984_12
특허 번호
US04490380

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