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Potassium Carbonate → HCID 131728130、化合物

HRID 2238682
ノート
印刷プレビュー

反応式

HRID 2238682 の反応式
CC1(C)C(C)(C)OB([C:9]2[CH2:10][CH2:11][N:12]([C:15](=[O:20])[C:16]([F:19])([F:18])[F:17])[CH2:13][CH:14]=2)O1.[C:22]([O:26][C:27](=[O:38])[NH:28][C@H:29]([C:31]1[CH:36]=[CH:35][C:34](Br)=[CH:33][CH:32]=1)[CH3:30])([CH3:25])([CH3:24])[CH3:23].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O.C(OCC)(=O)C.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]>[C:22]([O:26][C:27](=[O:38])[NH:28][C@H:29]([C:31]1[CH:32]=[CH:33][C:34]([C:9]2[CH2:10][CH2:11][N:12]([C:15](=[O:20])[C:16]([F:17])([F:18])[F:19])[CH2:13][CH:14]=2)=[CH:35][CH:36]=1)[CH3:30])([CH3:23])([CH3:24])[CH3:25]
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 3

HCID 11430Potassium CarbonateHCID 56973617(S)-tert-Butyl (1-(4-bromophenyl)ethyl)carbamateHCID 713023762,2,2-trifluoro-1-(4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-5,6-dihydropyridin-1(2H)-yl)ethanone

生成物 1

HCID 131728130HCID 131728130、化合物収率 38.4%

試薬・触媒・溶媒 3

HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
触媒
HCID 6228Dimethylformamide溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

400 mg of the 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1-(trifluoroacetyl)-1,2,3,6-tetrahydropyridine [154-2] was dissolved in 10 mL of N,N-dimethylformamide, then 196 mg of the t-butyl[(1S)-1-(4-bromophenyl)ethyl]carbamate [106-1], 54 mg of [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium (II), and 181 mg of potassium carbonate were added thereto, and stirred overnight at 80° C. The reaction mixture was cooled back to room temperature, then diluted in 100 mL of ethyl acetate, and washed with water and saturated brine in the subsequent order. The obtained organic layer was dried over anhydrous magnesium sulfate, and the insolubles were filtered. The filtrate was concentrated under reduced pressure, and the obtained residue was purified by silica gel column chromatography, to obtain 100 mg of t-butyl((1S)-1-{4-[1-(trifluoroacetyl)-1,2,3,6-tetrahydropyridin-4-yl]phenyl}ethyl)carbamate [154-3] as a white solid.

後処理

  1. temperatureThe reaction mixture was cooled back to room temperature
  2. washwashed with water and saturated brine in the subsequent order
  3. dry with materialThe obtained organic layer was dried over anhydrous magnesium sulfate
  4. filtrationthe insolubles were filtered
  5. concentrationThe filtrate was concentrated under reduced pressure
  6. customthe obtained residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-743e3e379bbb4b71851eb4845ed4a9ce
出典データセット
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07718801B2

反応ノート

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