Triphenylphosphine → 2-methyl-2-(4-nitro-1H-pyrazol-1-yl)propan-1-amine

HRID 714834노트

반응식

HRID 714834 반응식
[N:1]([CH2:4][C:5]([N:8]1[CH:12]=[C:11]([N+:13]([O-:15])=[O:14])[CH:10]=[N:9]1)([CH3:7])[CH3:6])=[N+]=[N-].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>O1CCCC1.O>[CH3:7][C:5]([N:8]1[CH:12]=[C:11]([N+:13]([O-:15])=[O:14])[CH:10]=[N:9]1)([CH3:6])[CH2:4][NH2:1]

참가 물질

4

반응물 2

HCID 11776TriphenylphosphineHCID 1178402371-(1-azido-2-methylpropan-2-yl)-4-nitro-1H-pyrazole

생성물 1

HCID 825041082-methyl-2-(4-nitro-1H-pyrazol-1-yl)propan-1-amine수율 99.3%

시약·촉매·용매 1

HCID 21881883Oxolane--water (1/1)용매

실험 절차

To a solution of 1-(1-azido-2-methylpropan-2-yl)-4-nitro-1H-pyrazole (10 g) obtained in Step C of Example 115 in a mixed solvent of tetrahydrofuran/water (v/v=10/1, 88 mL) was added triphenylphosphine (15 g), and the mixture was stirred overnight at room temperature. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/methanol) to give the title compound (8.7 g) as a mixture with triphenylphosphine oxide.

후처리

  1. customThe solvent was evaporated under reduced pressure
  2. customthe residue was purified by silica gel column chromatography (ethyl acetate/methanol)

출처 및 근거

ORD 기록
ord-f42104d714724122bd1f495aca85cfbd
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09187453B2

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