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Potassium Carbonate → 1,1-dimethylethyl 4-({4-[(2S,4R)-1-acetyl-2-methyl-4-({[(1-methylethyl)oxy]carbonyl}amino)-1,2,3,4-tetrahydro-6-quinolinyl]phenyl}methyl)-3-oxo-1-piperazinecarboxylate

HRID 2366867
ノート
印刷プレビュー

反応式

HRID 2366867 の反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([CH2:8][N:9]2[CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:11][C:10]2=[O:22])=[CH:4][CH:3]=1.[CH3:23][CH:24]([O:26][C:27](=[O:52])[NH:28][C@H:29]1[C:38]2[C:33](=[CH:34][CH:35]=[C:36](B3OC(C)(C)C(C)(C)O3)[CH:37]=2)[N:32]([C:48](=[O:50])[CH3:49])[C@@H:31]([CH3:51])[CH2:30]1)[CH3:25].C(=O)([O-])[O-].[K+].[K+].O1CCOCC1>C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].O>[C:48]([N:32]1[C:33]2[C:38](=[CH:37][C:36]([C:2]3[CH:7]=[CH:6][C:5]([CH2:8][N:9]4[CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:11][C:10]4=[O:22])=[CH:4][CH:3]=3)=[CH:35][CH:34]=2)[C@H:29]([NH:28][C:27]([O:26][CH:24]([CH3:25])[CH3:23])=[O:52])[CH2:30][C@@H:31]1[CH3:51])(=[O:50])[CH3:49]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 11430Potassium CarbonateHCID 312751,4-DioxaneHCID 67196654Tert-butyl 4-[(4-bromophenyl)methyl]-3-oxopiperazine-1-carboxylateHCID 681853941-Methylethyl [(cis)-1-acetyl-2-methyl-6-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1,2,3,4-tetrahydro-4-quinolinyl]carbamate

生成物 1

HCID 67195489
1,1-dimethylethyl 4-({4-[(2S,4R)-1-acetyl-2-methyl-4-({[(1-methylethyl)oxy]carbonyl}amino)-1,2,3,4-tetrahydro-6-quinolinyl]phenyl}methyl)-3-oxo-1-piperazinecarboxylate
収率 104%

試薬・触媒・溶媒 2

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)触媒HCID 962Water溶媒

反応条件

温度
120 °C

実験手順

A flask was charged with 1,1-dimethylethyl 4-[(4-bromophenyl)methyl]-3-oxo-1-piperazinecarboxylate (for a preparation, see Intermediate 72) (111 mg, 0.3 mmol), 1-methylethyl[(2S,4R)-1-acetyl-2-methyl-6-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1,2,3,4-tetrahydro-4-quinolinyl]carbamate (for a preparation, see Intermediate 52) (250 mg, 0.600 mmol), potassium carbonate (124 mg, 0.900 mmol) and [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (21.95 mg, 0.030 mmol) then filled with 1,4-dioxane (3 mL) and water (1 mL) and flushed with nitrogen. The resulting mixture was stirred under microwave irradiation at 120° C. for 30 min then cooled to room temperature. Most of the 1,4-dioxane was removed in vacuo and the residue was partitioned between AcOEt and water. The layers were separated and the aqueous phase was extracted with AcOEt. The combined organic phases were washed with brine, dried over MgSO4 and concentrated in vacuo. Purification of the residue by SP4 using a 25 G silica cartridge (gradient: 5 to 25% (10% MeOH in DCM) in DCM) gave 1,1-dimethylethyl 4-({4-[(2S,4R)-1-acetyl-2-methyl-4-({[(1-methylethyl)oxy]carbonyl}amino)-1,2,3,4-tetrahydro-6-quinolinyl]phenyl}methyl)-3-oxo-1-piperazinecarboxylate (180 mg, 0.311 mmol, 104% yield) which was used in the next step without further purification.

後処理

  1. customfor a preparation
  2. customfor a preparation
  3. customflushed with nitrogen
  4. temperaturethen cooled to room temperature
  5. customMost of the 1,4-dioxane was removed in vacuo
  6. customthe residue was partitioned between AcOEt and water
  7. customThe layers were separated
  8. extractionthe aqueous phase was extracted with AcOEt
  9. washThe combined organic phases were washed with brine
  10. dry with materialdried over MgSO4
  11. concentrationconcentrated in vacuo
  12. customPurification of the residue by SP4

出典と根拠

ORDレコード
ord-ce04cd9fee08475aa5a7d3451acb5bc2
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08697725B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート