4-Fluorophenyl isocyanate → HCID 178463336、化合物

HRID 1943491

反応式

HRID 1943491 の反応式
[NH2:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([NH:8][C:9]2[CH:10]=[C:11]([NH:28][CH2:29][CH3:30])[C:12]3[N:13]([C:15]([C:18]([NH:20][C:21]4[CH:26]=[CH:25][N:24]=[CH:23][C:22]=4[F:27])=[O:19])=[CH:16][N:17]=3)[N:14]=2)[CH2:4][CH2:3]1.[F:31][C:32]1[CH:37]=[CH:36][C:35]([N:38]=[C:39]=[O:40])=[CH:34][CH:33]=1>C1COCC1>[CH2:29]([NH:28][C:11]1[C:12]2[N:13]([C:15]([C:18]([NH:20][C:21]3[CH:26]=[CH:25][N:24]=[CH:23][C:22]=3[F:27])=[O:19])=[CH:16][N:17]=2)[N:14]=[C:9]([NH:8][C@H:5]2[CH2:4][CH2:3][C@H:2]([NH:1][C:39](=[O:40])[NH:38][C:35]3[CH:36]=[CH:37][C:32]([F:31])=[CH:33][CH:34]=3)[CH2:7][CH2:6]2)[CH:10]=1)[CH3:30]

参加物

4

反応物 2

HCID 709554-Fluorophenyl isocyanateHCID 178463334HCID 178463334、化合物

生成物 1

HCID 178463336HCID 178463336、化合物収率 78.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To suspension of 82B (20 mg, 0.048 mmol) in THF was added 4-fluorophenylisocyanate (6.54 μL, 0.058 mmol). The mixture was stirred at room temperature overnight. The solvent was removed under reduced and MeOH (1 mL) was added. The mixture was sonicated and the solid was collected by filtration, rinsed with a small amount of MeOH and dried under vacuum to give 8-(ethylamino)-6-((trans-4-(((4-fluorophenyl)carbamoyl)amino)cyclohexyl)amino)-N-(3-fluoro-4-pyridinyl)imidazo[1,2-b]pyridazine-3-carboxamide (20.8 mg) as an off white solid. HPLC Rt=3.176 minutes (Chromolith SpeedROD 4.6×50 mm, 10-90% aqueous methanol containing 0.1% TFA, 4 min gradient, monitored at 220 nm). [M+H]=550.

後処理

  1. customThe solvent was removed
  2. additionMeOH (1 mL) was added
  3. customThe mixture was sonicated
  4. filtrationthe solid was collected by filtration
  5. washrinsed with a small amount of MeOH
  6. customdried under vacuum

出典と根拠

ORDレコード
ord-3b38bde6195d461eae3cc7aa0b958dba
出典データセット
uspto-grants-2013_03
特許番号
US08389527B2

関連ノート

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