5-(2,2-Difluoroethyl)-2-nitro-4,5,6,7-tetrahydropyrazolo[1,5-a]pyrazine → 5-(2,2-Difluoroethyl)-4,5,6,7-tetrahydropyrazolo[1,5-a]pyrazin-2-amine
反応式
[F:1][CH:2]([F:16])[CH2:3][N:4]1[CH2:9][CH2:8][N:7]2[N:10]=[C:11]([N+:13]([O-])=O)[CH:12]=[C:6]2[CH2:5]1.[H][H]>C(O)C.[Pd]>[F:16][CH:2]([F:1])[CH2:3][N:4]1[CH2:9][CH2:8][N:7]2[N:10]=[C:11]([NH2:13])[CH:12]=[C:6]2[CH2:5]1参加物
5
実験手順
A solution of 135a (370 mg, 1.59 mmol) in ethanol (20 mL) was added Pd/C (about 200 mg). The reaction was charged with hydrogen gas (via balloon) and stirred at room temperature for 2 h. After reaction was complete, the mixture was filtered through a plug of CELITE®. The filtrate was concentrated reduced pressure to afford 135b as a yellow solid (293 mg, 91%), which was used in the next step without further purification. MS-ESI: [M+H]+ 203.2
後処理
- customAfter reaction
- filtrationthe mixture was filtered through a plug of CELITE®
- concentrationThe filtrate was concentrated reduced pressure
出典と根拠
- ORDレコード
- ord-be1ef488aa1a402789dd3eb6a1c40509
- 出典データセット
- uspto-grants-2014_06
- 特許番号
- US08754077B2
反応ノート
読み込み中…