HCID 59452727、化合物 → HCID 59452788、化合物

HRID 419638

反応式

HRID 419638 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([N+:8]([O-])=O)[C:5]([O:11][CH3:12])=[CH:4][C:3]=1[N:13]1[CH2:18][CH2:17][N:16]([S:19]([CH3:22])(=[O:21])=[O:20])[CH2:15][CH2:14]1>CCOC(C)=O.CO.C(Cl)Cl>[CH3:1][C:2]1[C:3]([N:13]2[CH2:18][CH2:17][N:16]([S:19]([CH3:22])(=[O:20])=[O:21])[CH2:15][CH2:14]2)=[CH:4][C:5]([O:11][CH3:12])=[C:6]([CH:7]=1)[NH2:8]

参加物

3

反応物 1

HCID 59452727HCID 59452727、化合物

生成物 1

HCID 59452788HCID 59452788、化合物収率 76.1%

試薬・触媒・溶媒 1

HCID 21901258Dichloromethane ethyl acetate methanol溶媒

実験手順

1-[2-methyl-5-(methyloxy)-4-nitrophenyl]-4-(methylsulfonyl)piperazine (0.87 g, 2.64 mmol) was placed in a 100 mL high pressure vessel and dissolved in 60 mL of 1 to 1 to 1 EtOAc/MeOH/DCM. 5 wt % Platinum(sulfided)/C (1.03 g, 0.26 mmol) was added followed quickly by a rubber septum. The vessel was evacuated and filled with N2 six times to remove any oxygen. The vessel was then pressurized with H2 (60 psi). The solution stirred overnight. The next morning the vessel was evacuated and filled with N2 six times to remove any H2. The solution was filtered through celite and evaporated to afford the title compound of step B (0.602 g, 2.01 mmol, 76%). 1H NMR (400 MHz, DMSO-d6) δ ppm 6.58 (s, 1H), 6.43 (s, 1H), 4.44 (s, 2H), 3.69 (s, 3H), 3.15-3.23 (m, 4H), 2.90 (s, 3H), 2.77-2.83 (m, 4H), 2.06 (s, 3H).

後処理

  1. customThe vessel was evacuated
  2. additionfilled with N2 six times
  3. customto remove any oxygen
  4. customThe next morning the vessel was evacuated
  5. additionfilled with N2 six times
  6. customto remove any H2
  7. filtrationThe solution was filtered through celite
  8. customevaporated

出典と根拠

ORDレコード
ord-d32f5ea37b6548bda6f89e4ac3b28985
出典データセット
uspto-grants-2012_01
特許番号
US08093239B2

関連ノート

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