5-Nitro-2-(4-(oxetan-3-yl)piperazin-1-yl)benzonitrile → HCID 86704502、化合物

HRID 633405ノート

反応式

HRID 633405 の反応式
[N+:1]([C:4]1[CH:5]=[CH:6][C:7]([N:12]2[CH2:17][CH2:16][N:15]([CH:18]3[CH2:21][O:20][CH2:19]3)[CH2:14][CH2:13]2)=[C:8]([CH:11]=1)[C:9]#[N:10])([O-])=O>CCO.[Pd]>[NH2:1][C:4]1[CH:5]=[CH:6][C:7]([N:12]2[CH2:17][CH2:16][N:15]([CH:18]3[CH2:19][O:20][CH2:21]3)[CH2:14][CH2:13]2)=[C:8]([CH:11]=1)[C:9]#[N:10]

参加物

4

反応物 1

HCID 867045015-Nitro-2-(4-(oxetan-3-yl)piperazin-1-yl)benzonitrile

生成物 1

HCID 86704502HCID 86704502、化合物収率 93%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

A mixture of 5-nitro-2-(4-(oxetan-3-yl)piperazin-1-yl)benzonitrile (9.8 g, 1.0 eq, 34.0 mmol) and Pd—C (10% loading, 3,6 g) in EtOH (300 mL) was stirred in a 500 mL round bottom flask. The reaction flask was evacuated under house vacuum and subsequently filled with hydrogen while stirring. This procedure was repeated three times and the reaction mixture was hydrogenated for 3 hours under an H2 balloon. The mixture was filtered through celite and the filter cake was washed with EtOH (2×50 mL). The filtrate was concentrated under vacuum to leave a white solid, which upon high vacuum drying gave 5-amino-2-(4-(oxetan-3-yl)piperazin-1-yl)benzonitrile in 93% yield.

後処理

  1. customThe reaction flask was evacuated under house vacuum
  2. additionsubsequently filled with hydrogen
  3. stirringwhile stirring
  4. filtrationThe mixture was filtered through celite
  5. washthe filter cake was washed with EtOH (2×50 mL)
  6. concentrationThe filtrate was concentrated under vacuum
  7. customto leave a white solid, which upon high vacuum
  8. customdrying

出典と根拠

ORDレコード
ord-5af8b77e67b4431da779fee981452691
出典データセット
uspto-grants-2016_04
特許番号
US09321763B2

反応ノート

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