5-Nitro-2-(4-(oxetan-3-yl)piperazin-1-yl)benzonitrile → HCID 86704502, 화합물

HRID 633405노트

반응식

HRID 633405 반응식
[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]

참가 물질

4

반응물 1

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

생성물 1

HCID 86704502HCID 86704502, 화합물수율 93%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5af8b77e67b4431da779fee981452691
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09321763B2

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