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Morpholine → (+/-)-tert-Butyl 4-(4-fluorophenyl)-4-((1-(5-morpholino-2-((2-(trimethylsilyl)ethoxy)methyl)-2H-indazol-7-yl)ethoxy)methyl)piperidine-1-carboxylate

HRID 913854
ノート
印刷プレビュー

反応式

HRID 913854 の反応式
Br[C:2]1[CH:10]=[C:9]([CH:11]([O:13][CH2:14][C:15]2([C:28]3[CH:33]=[CH:32][C:31]([F:34])=[CH:30][CH:29]=3)[CH2:20][CH2:19][N:18]([C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[CH2:17][CH2:16]2)[CH3:12])[C:8]2[C:4](=[CH:5][N:6]([CH2:35][O:36][CH2:37][CH2:38][Si:39]([CH3:42])([CH3:41])[CH3:40])[N:7]=2)[CH:3]=1.CC(C)([O-])C.[Na+].C(N1CCN2CCN(CC(C)C)P1N(CC(C)C)CC2)C(C)C.[NH:72]1[CH2:77][CH2:76][O:75][CH2:74][CH2:73]1>C1(C)C=CC=CC=1.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[F:34][C:31]1[CH:32]=[CH:33][C:28]([C:15]2([CH2:14][O:13][CH:11]([C:9]3[C:8]4[C:4](=[CH:5][N:6]([CH2:35][O:36][CH2:37][CH2:38][Si:39]([CH3:42])([CH3:41])[CH3:40])[N:7]=4)[CH:3]=[C:2]([N:72]4[CH2:77][CH2:76][O:75][CH2:74][CH2:73]4)[CH:10]=3)[CH3:12])[CH2:20][CH2:19][N:18]([C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[CH2:17][CH2:16]2)=[CH:29][CH:30]=1
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 8083MorpholineHCID 45712432,8,9-Triisobutyl-2,5,8,9-tetraaza-1-phosphabicyclo(3.3.3)undecaneHCID 23676156Sodium t-butoxideHCID 57546111(+/-)-tert-Butyl 4-((1-(5-bromo-2-((2-(trimethylsilyl)ethoxy)methyl)-2H-indazol-7-yl)ethoxy)methyl)-4-(4-fluorophenyl)piperidine-1-carboxylate

生成物 1

HCID 57546046
(+/-)-tert-Butyl 4-(4-fluorophenyl)-4-((1-(5-morpholino-2-((2-(trimethylsilyl)ethoxy)methyl)-2H-indazol-7-yl)ethoxy)methyl)piperidine-1-carboxylate

試薬・触媒・溶媒 2

HCID 167845palladium(II) acetate触媒HCID 1140Toluene溶媒

反応条件

温度
100 °C

実験手順

(±)-tert-Butyl 4-((1-(5-bromo-2-((2-(trimethylsilyl)ethoxy)methyl)-2H-indazol-7-yl)ethoxy)methyl)-4-(4-fluorophenyl)piperidine-1-carboxylate (75 mg, 0.113 mmol), sodium tert-butoxide (16.3 mg, 0.17 mmol), and palladium(II)acetate (1.02 mg, 4.53 μmol) were combined in toluene (2 mL) and treated with 2,8,9-triisobutyl-2,5,8,9-tetraaza-1-phosphabicyclo[3.3.3]undecane (3.1 mg, 9.05 μmol) and morpholine (0.012 mL, 0.136 mmol) in a microwave tube and sealed. After flushing the mixture with nitrogen, the mixture was heated at 100° C. for 1 h via microwave. After cooling to room temperature, the reaction mixture was concentrated, dissolved in ethyl acetate, washed with water and brine, concentrated, and purified by flash chromatography on silica gel (30% EtOAc/Hex) to afford 44 mg (58%) as an oil. LC/MS (HPLC method 2): tR=3.185 min, 669.25(MH)+.

後処理

  1. customsealed
  2. customAfter flushing the mixture with nitrogen
  3. temperatureAfter cooling to room temperature
  4. concentrationthe reaction mixture was concentrated
  5. dissolutiondissolved in ethyl acetate
  6. washwashed with water and brine
  7. concentrationconcentrated
  8. custompurified by flash chromatography on silica gel (30% EtOAc/Hex)
  9. customto afford 44 mg (58%) as an oil

出典と根拠

ORDレコード
ord-52a9e670451a4a2b93bf033514d0aa83
出典データセット
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08026257B2

反応ノート

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