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Potassium Phosphate, Tribasic → [2-(2,6-Dichloro-4-cyanophenyl)-2H-pyrazolo[4,3-c]pyridin-4-yl]carbamic acid tert-butyl ester

HRID 626696
ノート
印刷プレビュー

反応式

HRID 626696 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([Cl:20])[C:9]=1[N:10]1[CH:19]=[C:13]2[C:14](Cl)=[N:15][CH:16]=[CH:17][C:12]2=[N:11]1)[C:5]#[N:6].[C:21](=[O:28])([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])[NH2:22].[O-]P([O-])([O-])=O.[K+].[K+].[K+]>C1(C)C=CC=CC=1.O.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].CC1(C)C2C(=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=CC=2)OC2C(P(C3C=CC=CC=3)C3C=CC=CC=3)=CC=CC1=2>[C:24]([O:23][C:21](=[O:28])[NH:22][C:14]1[C:13]2=[CH:19][N:10]([C:9]3[C:2]([Cl:1])=[CH:3][C:4]([C:5]#[N:6])=[CH:7][C:8]=3[Cl:20])[N:11]=[C:12]2[CH:17]=[CH:16][N:15]=1)([CH3:27])([CH3:26])[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

8

反応物 3

HCID 62657Potassium Phosphate, TribasicHCID 77922tert-Butyl carbamateHCID 866970463,5-Dichloro-4-(4-chloropyrazolo[4,3-c]pyridin-2-yl)benzonitrile

生成物 1

HCID 69674840[2-(2,6-Dichloro-4-cyanophenyl)-2H-pyrazolo[4,3-c]pyridin-4-yl]carbamic acid tert-butyl ester収率 123.7%

試薬・触媒・溶媒 4

HCID 636044
1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)
触媒
HCID 9811564Bis(dibenzylideneacetone)palladium触媒
HCID 962Water溶媒
HCID 1140Toluene溶媒

反応条件

温度
90 °C

実験手順

A mixture of 3,5-dichloro-4-(4-chloro-pyrazolo[4,3-c]pyridin-2-yl)-benzonitrile (3.23 g, 10 mmol), tert-butyl carbamate (5.85 mg, 50 mmol), Pd2(dba)3 (458 mg, 0.5 mmol), Xantphos (576 mg, 1.0 mmol) and potassium phosphate tribasic (4.24 g, 20 mmol) in toluene (100 mL) and water (20 mL) was degassed with argon then heated at 90° C. for 30 minutes. The reaction was cooled to room temperature and then filtered through Celite® using ethyl acetate to wash the filter pad. The filtrate was washed with water and sodium bicarbonate (sat. aq.), dried over sodium sulfate and concentrated under reduced pressure. The resultant residue was purified by silica gel flash chromatography (0-50% ethyl acetate in cyclohexane) to afford the title compound as an off-white solid (5.0 g, contaminated with residual tert-butyl carbamate). LCMS (Method D): RT=2.44 min, m/z: 348 [M−C4H7+].

後処理

  1. customwas degassed with argon
  2. temperatureThe reaction was cooled to room temperature
  3. filtrationfiltered through Celite®
  4. washto wash the filter pad
  5. washThe filtrate was washed with water and sodium bicarbonate (sat. aq.)
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe resultant residue was purified by silica gel flash chromatography (0-50% ethyl acetate in cyclohexane)

出典と根拠

ORDレコード
ord-5ad18958b62b4ec4b687a774e62bd8da
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09309240B2

反応ノート

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