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Dichloromethane → HCID 18446586、化合物

HRID 1868329
ノート
印刷プレビュー

反応式

HRID 1868329 の反応式
[C:1]([C:3]1[C:4]2[S:12][C:11](Br)=[CH:10][C:5]=2[C:6](=[O:9])[NH:7][CH:8]=1)#[N:2].[C:14]([C:18]1[CH:23]=[CH:22][C:21](B(O)O)=[CH:20][CH:19]=1)([CH3:17])([CH3:16])[CH3:15].C(=O)([O-])[O-].[K+].[K+].ClCCl>CN(C=O)C.O.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:1]([C:3]1[C:4]2[S:12][C:11]([C:21]3[CH:22]=[CH:23][C:18]([C:14]([CH3:17])([CH3:16])[CH3:15])=[CH:19][CH:20]=3)=[CH:10][C:5]=2[C:6](=[O:9])[NH:7][CH:8]=1)#[N:2]
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 4

HCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 27343204-tert-Butylphenylboronic acidHCID 184465192-Bromo-4-oxo-4,5-dihydrothieno[3,2-c]pyridine-7-carbonitrile

生成物 1

HCID 18446586HCID 18446586、化合物収率 57.9%

試薬・触媒・溶媒 3

HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
触媒
HCID 962Water溶媒
HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
80 °C

実験手順

To a solution of 7-cyano-2-bromo-4-oxo-4,5-dihydrothieno[3,2-c]-pyridine (2.0 g, 7.84 mmol) in DMF (40 mL) and water (15 mL) was added 4-t-butylphenyl boronic acid (2.1 g, 11.8 mmol), potassium carbonate (1.4 g, 10.1 mmol) and [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II), complex with dichloromethane (1:1) (0.192 g, 0.23 mmol). The resulting mixture was stirred under nitrogen for 4 h at 80° C. After this time the mixture was diluted with DMF (20 mL), filtered through celite to remove palladium residues and water (100 mL) added. The precipitated solid was filtered, washed thoroughly with water and dried in air by suction at room temperature providing 1.4 g of 100 which was used without further analysis or purification.

後処理

  1. filtrationfiltered through celite
  2. customto remove palladium residues and water (100 mL)
  3. additionadded
  4. filtrationThe precipitated solid was filtered
  5. washwashed thoroughly with water
  6. customdried in air by suction at room temperature

出典と根拠

ORDレコード
ord-251758f11325475995ea83627c83fe3d
出典データセット
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07635695B2

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