Ammonia → HCID 13151408、化合物

HRID 851277ノート

反応式

HRID 851277 の反応式
[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

参加物

4

反応物 2

HCID 222AmmoniaHCID 20501992HCID 20501992、化合物

生成物 1

HCID 13151408HCID 13151408、化合物収率 28%

試薬・触媒・溶媒 1

HCID 713Formamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b742a7aeaa3d488897d7f6102eb1b21d
出典データセット
uspto-grants-1983_05
特許番号
US04383851

反応ノート

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