HCID 14770832, 화합물 → HCID 14770833, 화합물

HRID 1651573노트

반응식

HRID 1651573 반응식
[Br:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([C:9]2[CH2:13][CH2:12][C:11](=[O:14])[CH:10]=2)=[C:4]([F:15])[CH:3]=1>C1COCC1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.[Cl-].[Rh]>[Br:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([CH:9]2[CH2:13][CH2:12][C:11](=[O:14])[CH2:10]2)=[C:4]([F:15])[CH:3]=1

참가 물질

4

반응물 1

HCID 14770832HCID 14770832, 화합물

생성물 1

HCID 14770833HCID 14770833, 화합물수율 93%

시약·촉매·용매 2

HCID 84599Chlorotris(triphenylphosphine)rhodium(I)촉매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 16.4 g (60.2 mmol) of 3-(4-bromo-2,5-difluorophenyl)-2-cyclopentenone in 400 ml of THF was hydrogenated over 2.0 g of Wilkinson's catalyst at 25° C. for 18 hours. The solution was concentrated to a brown oil which was chromatographed on silica gel (E. Merck-230-400 Mesh) to remove the catalyst. The residue obtained was triturated with hexane, and the solids were filtered, washed with hexane, and dried to give 15.2 g (93%) of the title compound; mp 63°-65° C.

후처리

  1. concentrationThe solution was concentrated to a brown oil which
  2. customwas chromatographed on silica gel (E. Merck-230-400 Mesh)
  3. customto remove the catalyst
  4. customThe residue obtained
  5. customwas triturated with hexane
  6. filtrationthe solids were filtered
  7. washwashed with hexane
  8. customdried

출처 및 근거

ORD 기록
ord-45b4290656ff4535a3d91d802e9a44ef
출처 데이터셋
uspto-grants-1990_05
특허 번호
US04929613

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