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Hydrochloric Acid → 5-Fluoropyridine-2,4-diaminehydrochloride

HRID 610237
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HRID 610237 반응식
[ClH:1].C([NH:9][C:10]1[CH:15]=[C:14]([NH2:16])[C:13]([F:17])=[CH:12][N:11]=1)C1C=CC=CC=1>[Pd].CO>[ClH:1].[NH2:9][C:10]1[CH:15]=[C:14]([NH2:16])[C:13]([F:17])=[CH:12][N:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 221212872-Benzylamino-4-amino-5-fluoropyridine

생성물 1

HCID 221212585-Fluoropyridine-2,4-diaminehydrochloride수율 98.7%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

To 4 ml of methanol having added 400 mg of concentrated hydrochloric acid added thereto was added 350 mg of 2-benzylamino-4-amino-5-fluoropyridine together with 50 mg of 10% palladium on carbon, and the mixture was hydrogenated at 40° C. for 2 days. The catalyst was separated by filtration, and the solvent and the like were distilled off under reduced pressure. Procedure of adding 10 ml of distilled water to the residue and concentrating under reduced pressure was repeated 4 times, and the procedure of adding 10 ml of ethanol and concentrating under reduced pressure was repeated twice. 260 mg of the title compound was obtained as a residue in the form of a yellowish orange paste.

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후처리

  1. additionadded
  2. customThe catalyst was separated by filtration
  3. distillationthe solvent and the like were distilled off under reduced pressure
  4. additionProcedure of adding 10 ml of distilled water to the residue
  5. concentrationconcentrating under reduced pressure
  6. additionthe procedure of adding 10 ml of ethanol
  7. concentrationconcentrating under reduced pressure

출처 및 근거

ORD 기록
ord-11c8ba0c99d746d0a02e1644b67a8cda
출처 데이터셋
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05998436

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