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1,3-Dibromobenzene → tert-Butyl 4-{3-[(3-bromophenyl)amino]-4-carbamoyl-1H-pyrazol-1-yl}-4-(cyanomethyl)piperidine-1-carboxylate

HRID 521219
ノート
印刷プレビュー

反応式

HRID 521219 の反応式
[NH2:1][C:2]1[C:6]([C:7](=[O:9])[NH2:8])=[CH:5][N:4]([C:10]2([CH2:23][C:24]#[N:25])[CH2:15][CH2:14][N:13]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:12][CH2:11]2)[N:3]=1.C([O-])(=O)C.[K+].[Br:31][C:32]1[CH:37]=[CH:36][CH:35]=[C:34](Br)[CH:33]=1.C(P(C(C)(C)C)C1C(C)=C(C)C(C)=C(C)C=1C1C(C(C)C)=CC(C(C)C)=CC=1C(C)C)(C)(C)C>C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].CC(O)C>[Br:31][C:32]1[CH:33]=[C:34]([NH:1][C:2]2[C:6]([C:7](=[O:9])[NH2:8])=[CH:5][N:4]([C:10]3([CH2:23][C:24]#[N:25])[CH2:15][CH2:14][N:13]([C:16]([O:18][C:19]([CH3:20])([CH3:21])[CH3:22])=[O:17])[CH2:12][CH2:11]3)[N:3]=2)[CH:35]=[CH:36][CH:37]=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 79271,3-DibromobenzeneHCID 517044Potassium AcetateHCID 11953610Di-tert-butyl[3,4,5,6-tetramethyl-2',4',6'-tris(propan-2-yl)-[1,1'-biphenyl]-2-yl]phosphaneHCID 86729368tert-Butyl 4-(3-amino-4-carbamoyl-1H-pyrazol-1-yl)-4-(cyanomethyl)piperidine-1-carboxylate2 回

生成物 1

HCID 86729380
tert-Butyl 4-{3-[(3-bromophenyl)amino]-4-carbamoyl-1H-pyrazol-1-yl}-4-(cyanomethyl)piperidine-1-carboxylate

試薬・触媒・溶媒 2

HCID 9811564Bis(dibenzylideneacetone)palladium触媒HCID 3776Isopropanol溶媒

反応条件

温度
85 °C

実験手順

tert-Butyl 4-(3-amino-4-carbamoyl-1H-pyrazol-1-yl)-4-(cyanomethyl)piperidine-1-carboxylate (Intermediate 35-1) (500 mg, 1.44 mmol), potassium acetate (211 mg, 2.15 mmol), 1,3-dibromobenzene (0.69 mL, 5.74 mmol) and 2-propanol (7.2 mL) were combined in a vial and purged with a stream of N2 gas for 10 minutes. Pd2(dba)3 (52 mg, 0.060 mmol) and 2-di-t-butylphosphino-3,4,5,6-tetramethyl-2′,4′,6′-tri-i-propylbiphenyl (103 mg, 0.220 mmol) were then added. The reaction vessel was capped and the reaction mixture was heated to 85° C. and allowed to stir for 16 hours. The mixture was then cooled to ambient temperature, filtered through celite, eluting with EtOAc. The filtrate was concentrated in vacuo and the residue was purified by MPLC on silica gel (using a gradient elution of 0-10% MeOH/DCM) to afford the title compound, Example #12-1.

後処理

  1. custompurged with a stream of N2 gas for 10 minutes
  2. customThe reaction vessel was capped
  3. temperatureThe mixture was then cooled to ambient temperature
  4. filtrationfiltered through celite
  5. washeluting with EtOAc
  6. concentrationThe filtrate was concentrated in vacuo
  7. customthe residue was purified by MPLC on silica gel (
  8. washa gradient elution of 0-10% MeOH/DCM)

出典と根拠

ORDレコード
ord-2b88f3959f694078af9bcb63a6238c63
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09328099B2

反応ノート

読み込み中…

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