Ammonia → HCID 13151408, 화합물

HRID 851277노트

반응식

HRID 851277 반응식
[NH3:1].[F:2][C:3]1[C:8]([C:9]([O:11][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[O:10])=[CH:7][CH:6]=[C:5](F)[N:4]=1>C(N)=O>[NH2:1][C:5]1[N:4]=[C:3]([F:2])[C:8]([C:9]([O:11][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[O:10])=[CH:7][CH:6]=1

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 20501992HCID 20501992, 화합물

생성물 1

HCID 13151408HCID 13151408, 화합물수율 28%

시약·촉매·용매 1

HCID 713Formamide용매

실험 절차

To a stirred solution of ammonia (15 g) in formamide (250 ml) was added all at once benzyl 2,6-difluoropyridine-3-carboxylate (20 g, 0.08 mole). The mixture slowly became homogeneous, then a solid began to separate. After two hours, the mixture was poured into water (1000 ml) and the solid filtered. The solid was washed with several portions of water then air dried. Continuous extraction for one hour via a Soxhlet extraction apparatus using hexane as the solvent gave, after concentrating to 250 ml and cooling, 6.0 g (30%) of the desired benzyl 2-amino-6-fluoropyridine-3-carboxylate: m.p.=92°-94° C. The hexane insoluble material was recrystallized from a small volume of acetone to give 5.5 g (28%) of the isomeric benzyl 6-amino-2-fluoropyridine-3-carboxylate: m.p.=157.5°-159.5° C.

후처리

  1. customto separate
  2. additionthe mixture was poured into water (1000 ml)
  3. filtrationthe solid filtered
  4. washThe solid was washed with several portions of water
  5. customair dried
  6. extractionContinuous extraction for one hour
  7. extractionvia a Soxhlet extraction apparatus
  8. customgave
  9. concentrationafter concentrating to 250 ml
  10. temperaturecooling
  11. customThe hexane insoluble material was recrystallized from a small volume of acetone

출처 및 근거

ORD 기록
ord-b742a7aeaa3d488897d7f6102eb1b21d
출처 데이터셋
uspto-grants-1983_05
특허 번호
US04383851

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