Hydrochloric Acid → HCID 20083098, 화합물

HRID 1656739노트

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HRID 1656739 반응식
N[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[C:4]([CH2:11][CH2:12][OH:13])[C:3]=1[F:14].[ClH:15].N([O-])=O.[Na+]>C(O)(=O)C>[Cl:15][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[C:4]([CH2:11][CH2:12][OH:13])[C:3]=1[F:14]

참가 물질

5

반응물 3

HCID 313Hydrochloric Acid3회HCID 207922134-Amino-3-fluoro-2-(2-hydroxyethyl)nitrobenzeneHCID 23668193Sodium Nitrite

생성물 1

HCID 20083098HCID 20083098, 화합물수율 83%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

7.33 g (37 mmol) of the compound (124) obtained in Reference Example 6 was added to 60 ml of 6N hydrochloric acid, and while cooling on ice, 15 ml of aqueous solution containing 2.95 g (43 mmol) of sodium nitrite was dropped to the solution through 5 minutes. The solution was stirred for 30 minutes as was. Then, 20 ml of concentrated hydrochloric acid and 20 ml of acetic acid were added to the solution, and the solution was stirred for 1 hour. While cooling on ice, 35 ml of concentrated hydrochloric acid solution containing 6.20 g (63 mmol) of cuprous chloride was dropped to the solution through 40 minutes, and the solution was stirred for 3 hours as was. The solution was extracted with 300 ml of ethyl acetate, and after drying over magnesium sulfate, the solvent was removed by distillation. The residue was separated by the column chromatography (silica gel 100 g, eluent solvent; chloroform:methanol=50:1) to obtain 6.69 g of the subject compound (125) in a 83% yield.

후처리

  1. additionwas dropped to the solution through 5 minutes
  2. stirringthe solution was stirred for 1 hour
  3. additionwas dropped to the solution through 40 minutes
  4. stirringthe solution was stirred for 3 hours
  5. extractionThe solution was extracted with 300 ml of ethyl acetate
  6. dry with materialafter drying over magnesium sulfate
  7. customthe solvent was removed by distillation
  8. customThe residue was separated by the column chromatography (silica gel 100 g, eluent solvent; chloroform:methanol=50:1)

출처 및 근거

ORD 기록
ord-1b4b64b29c834fa2b016acabb1a794df
출처 데이터셋
uspto-grants-1993_10
특허 번호
US05254685

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