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

HRID 714834ノート

反応式

HRID 714834 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 21881883Oxolane--water (1/1)溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-f42104d714724122bd1f495aca85cfbd
出典データセット
uspto-grants-2015_11
特許番号
US09187453B2

反応ノート

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