4-Fluorophenyl isocyanate → HCID 178463336, 화합물

HRID 1943491

반응식

HRID 1943491 반응식
[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]

참가 물질

4

반응물 2

HCID 709554-Fluorophenyl isocyanateHCID 178463334HCID 178463334, 화합물

생성물 1

HCID 178463336HCID 178463336, 화합물수율 78.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3b38bde6195d461eae3cc7aa0b958dba
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08389527B2

연결된 노트

불러오는 중…