2,6-Diethylaniline → HCID 86653101、化合物

HRID 81970

反応式

HRID 81970 の反応式
[I:1][C:2]1[N:11]=[CH:10][C:9]2[CH2:8][CH2:7][C:6]3[C:12]([C:16]([O:18]CC)=O)=[N:13][N:14]([CH3:15])[C:5]=3[C:4]=2[N:3]=1.[OH-].[K+].C(N(C(C)C)C(C)C)C.F[B-](F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2C=CC=CC=2N=N1.[CH2:54]([C:56]1[CH:62]=[CH:61][CH:60]=[C:59]([CH2:63][CH3:64])[C:57]=1[NH2:58])[CH3:55]>C(O)C>[CH2:54]([C:56]1[CH:62]=[CH:61][CH:60]=[C:59]([CH2:63][CH3:64])[C:57]=1[NH:58][C:16]([C:12]1[C:6]2[CH2:7][CH2:8][C:9]3[CH:10]=[N:11][C:2]([I:1])=[N:3][C:4]=3[C:5]=2[N:14]([CH3:15])[N:13]=1)=[O:18])[CH3:55]

参加物

7

反応物 5

HCID 113692,6-DiethylanilineHCID 14797Potassium HydroxideHCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 44232943ethyl 8-iodo-1-methyl-4,5-dihydro-1H-pyrazolo[4,3-h]quinazoline-3-carboxylate

生成物 1

HCID 86653101HCID 86653101、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Ethyl 8-iodo-1-methyl-4,5-dihydro-1H-pyrazolo[4,3-h]quinazoline-3-carboxylate (4.0 g, 10.4 mmol) prepared as described in WO2004/104007 was dissolved in anhydrous ethanol (150 mL) and treated with potassium hydroxide (5.83 g, 104 mmol.) at RT for 24 hour. The white precipitate formed during the reaction was collected by filtration. The solid was then suspended in anhydrous dimethylformamide (5.0 mL) and treated with N-ethyl-N,N-diisopropylamine (10 ml) and O-(Benzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium tetrafluoroborate (TBTU) (4.5 g, 14.1 mmol). The mixture was then treated with 2,6-diethylaniline (2.3 ml, 14.1 mmol) and stirred at room temperature overnight. The solvent was removed under reduced pressure and the crude was purified by column chromatography to afford the title compound.

後処理

  1. customThe white precipitate formed during the reaction
  2. filtrationwas collected by filtration
  3. customThe solvent was removed under reduced pressure
  4. customthe crude was purified by column chromatography

出典と根拠

ORDレコード
ord-059465ba97fd4bd59d5555eae22fd6f4
出典データセット
uspto-grants-2014_09
特許番号
US08846701B2

関連ノート

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