Formic Acid → HCID 20071081, 화합물

HRID 981816노트

반응식

HRID 981816 반응식
Cl[C:2]1[CH:7]=[C:6]([NH:8][CH3:9])[C:5]([N+:10]([O-:12])=[O:11])=[C:4]([NH2:13])[CH:3]=1.C(O)=O>C(N(CC)CC)C.[Pd]>[NH2:13][C:4]1[CH:3]=[CH:2][CH:7]=[C:6]([NH:8][CH3:9])[C:5]=1[N+:10]([O-:12])=[O:11]

참가 물질

5

반응물 2

HCID 284Formic AcidHCID 20071066HCID 20071066, 화합물

생성물 1

HCID 20071081HCID 20071081, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8471Triethylamine용매

반응 조건

온도
80 °C

실험 절차

59.5 mg of palladium at a concentration of 10% on charcoal are added to 0.014 mole (2.8 g) of 4-chloro-2-amino-6-methylaminonitrobenzene in 5.3 ml of triethylamine, and 1.16 ml of formic acid are then run in dropwise. A high exothermicity is noted. The reaction mixture is heated to 80° C. for 40 minutes. After dilution of the reaction mixture with ethanol, the catalyst is removed by hot filtration. The filtrate, evaporated under reduced pressure, enables a dry extract to be obtained. After dilution of the dry extract with water, the expected product precipitates. After being filtered off and washed with water, the precipitate is dried under vacuum in the presence of phosphorus pentoxide. After two recrystallizations from isopropanol in order to remove a gum, the product melts at 70° C.

후처리

  1. customAfter dilution of the reaction mixture with ethanol, the catalyst is removed by hot filtration
  2. customThe filtrate, evaporated under reduced pressure
  3. extractionextract
  4. customto be obtained
  5. extractionAfter dilution of the dry extract with water
  6. customthe expected product precipitates
  7. filtrationAfter being filtered off
  8. washwashed with water
  9. dry with materialthe precipitate is dried under vacuum in the presence of phosphorus pentoxide
  10. customAfter two recrystallizations from isopropanol in order
  11. customto remove a gum

출처 및 근거

ORD 기록
ord-17d6ff2e51d34a8e9902539caf952d50
출처 데이터셋
uspto-grants-1991_02
특허 번호
US04992586

반응 노트

불러오는 중…