2-(1-isopropyl-3-methyl-1H-1,2,4-triazol-5-yl)-9-vinyl-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepine → 9-ethyl-2-(1-isopropyl-3-methyl-1H-1,2,4-triazol-5-yl)-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepine

HRID 886503ノート

反応式

HRID 886503 の反応式
[CH:1]([N:4]1[C:8]([C:9]2[N:10]=[C:11]3[C:17]4[CH:18]=[CH:19][C:20]([CH:22]=[CH2:23])=[CH:21][C:16]=4[O:15][CH2:14][CH2:13][N:12]3[CH:24]=2)=[N:7][C:6]([CH3:25])=[N:5]1)([CH3:3])[CH3:2]>C(O)C>[CH2:22]([C:20]1[CH:19]=[CH:18][C:17]2[C:11]3[N:12]([CH:24]=[C:9]([C:8]4[N:4]([CH:1]([CH3:2])[CH3:3])[N:5]=[C:6]([CH3:25])[N:7]=4)[N:10]=3)[CH2:13][CH2:14][O:15][C:16]=2[CH:21]=1)[CH3:23]

参加物

3

反応物 1

HCID 582046742-(1-isopropyl-3-methyl-1H-1,2,4-triazol-5-yl)-9-vinyl-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepine

生成物 1

HCID 582049249-ethyl-2-(1-isopropyl-3-methyl-1H-1,2,4-triazol-5-yl)-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepine収率 62.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2-(1-isopropyl-3-methyl-1H-1,2,4-triazol-5-yl)-9-vinyl-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepine from Example 447 (0.300 g, 0.894 mmol) was dissolved in ethanol (5 mL) and purged with N2. 10% Palladium on Carbon (0.1:0.9, Palladium:carbon black, 0.0952 g) was added. The resulting suspension was placed under vacuum followed by addition of H2 at atm pressure. This process was repeated three times to saturate the catalyst. The reaction was stirred for 18 hours at room temperature. The reaction mixture was filtered and concentrated to dryness. The crude product was purified using reverse phase chromatography to give 499 (0.189 g, 62.9% yield).

後処理

  1. custompurged with N2
  2. addition10% Palladium on Carbon (0.1:0.9, Palladium:carbon black, 0.0952 g) was added
  3. additionfollowed by addition of H2 at atm pressure
  4. concentrationto saturate the catalyst
  5. filtrationThe reaction mixture was filtered
  6. concentrationconcentrated to dryness
  7. customThe crude product was purified

出典と根拠

ORDレコード
ord-0c6f4bae27ed4bae83fdd1b0ebeba624
出典データセット
uspto-grants-2012_08
特許番号
US08242104B2

反応ノート

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