Hydrazine hydrate (1:1) → HCID 59850187、化合物

HRID 2064159ノート

反応式

HRID 2064159 の反応式
[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]

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 59850135HCID 59850135、化合物

生成物 1

HCID 59850187HCID 59850187、化合物収率 99%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒

反応条件

温度
45 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1ab1cafc6abd4e968ac2245e275613b6
出典データセット
uspto-grants-2012_10
特許番号
US08288412B2

反応ノート

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