Hydrazine hydrate (1:1) → HCID 59850187, 화합물

HRID 2064159노트

반응식

HRID 2064159 반응식
[Br:1][C:2]1[C:3]([C:24]([F:27])([F:26])[F:25])=[CH:4][C:5]([N+:21]([O-])=O)=[C:6]([NH:8][CH:9]2[CH2:14][CH2:13][N:12]([CH:15]3[CH2:20][CH2:19][O:18][CH2:17][CH2:16]3)[CH2:11][CH2:10]2)[CH:7]=1.O.NN>C(O)C.[Ni]>[Br:1][C:2]1[CH:7]=[C:6]([NH:8][CH:9]2[CH2:10][CH2:11][N:12]([CH:15]3[CH2:20][CH2:19][O:18][CH2:17][CH2:16]3)[CH2:13][CH2:14]2)[C:5]([NH2:21])=[CH:4][C:3]=1[C:24]([F:26])([F:25])[F:27]

참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 59850135HCID 59850135, 화합물

생성물 1

HCID 59850187HCID 59850187, 화합물수율 99%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매

반응 조건

온도
45 °C

실험 절차

A stirred suspension of N-[5-bromo-2-nitro-4-(trifluoromethyl)phenyl]-1-(tetrahydro-2H-pyran-4-yl)-4-piperidinamine (D54) (380 mg, 0.84 mmole) in ethanol (20 ml) at room temperature under argon was treated with Raney Nickel (20 mg) followed by the dropwise addition of hydrazine hydrate (0.25 ml, 8.0 mmole). The mixture was maintained at room temp. for 0.5 hr, then heated at 45° C. for 1 hr producing a grey solution, which was filtered through Kieselguhr and the filtrate concentrated under vacuum to afford the title compound as a pale yellow solid (350 mg, 99%). MH+=422, 424.

후처리

  1. temperatureThe mixture was maintained at room temp. for 0.5 hr
  2. customproducing a grey solution, which
  3. filtrationwas filtered through Kieselguhr
  4. concentrationthe filtrate concentrated under vacuum

출처 및 근거

ORD 기록
ord-1ab1cafc6abd4e968ac2245e275613b6
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08288412B2

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