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Triphenylphosphine → HCID 13341551, 화합물

HRID 542626
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HRID 542626 반응식
[N:1]([CH:4]1[CH2:16][N:7]2[CH2:8][CH2:9][CH2:10][CH:11]([C:12]([O:14]C)=[O:13])[N:6]2[C:5]1=[O:17])=[N+]=[N-].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>O1CCOCC1>[NH2:1][CH:4]1[CH2:16][N:7]2[CH2:8][CH2:9][CH2:10][CH:11]([C:12]([OH:14])=[O:13])[N:6]2[C:5]1=[O:17]
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참가 물질

4

반응물 2

HCID 11776TriphenylphosphineHCID 13341556HCID 13341556, 화합물

생성물 1

HCID 13341551HCID 13341551, 화합물수율 76.3%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

1.19 g of methyl 2-azido-hexahydro-3-oxo-1H-pyrazolo[1,2-a]pyridazine-5-carboxylate (racemate A) and 1.31 g of triphenylphosphine in 25 ml of dioxane were stirred at room temperature for 1 hour and the mixture was then evaporated. The residue was treated with 40 ml of 2N aqueous ammonia at 50° C. for 2.5 hours and the precipitated triphenyl phosphine oxide was removed by filtration. Evaporation then yielded 0.756 g (76%) of 2-amino-hexahydro-3-oxo-1H-pyrazolo[1,2-a]pyridazine-5-carboxylic acid (racemate A) in the form of a white solid which, after recrystallization from aqueous methanol, melted at 245°-246° C. (decomposition).

후처리

  1. customthe mixture was then evaporated
  2. additionThe residue was treated with 40 ml of 2N aqueous ammonia at 50° C. for 2.5 hours
  3. customthe precipitated triphenyl phosphine oxide was removed by filtration
  4. customEvaporation

출처 및 근거

ORD 기록
ord-4d19032148dd4200bed9fe3d5f4e1410
출처 데이터셋
uspto-grants-1987_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04658024

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