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Ethanol → HCID 68285965、化合物

HRID 1053276
ノート
印刷プレビュー

反応式

HRID 1053276 の反応式
[Br:1][C:2]1[C:6]([N:7]([CH3:9])[CH3:8])=[C:5](Br)[S:4][C:3]=1[C:11]([O:13][CH2:14][CH3:15])=[O:12].C(O)C.[Cl:19][C:20]1[CH:25]=[CH:24][C:23](B(O)O)=[CH:22][CH:21]=1.C(=O)([O-])[O-].[K+].[K+]>C1(C)C=CC=CC=1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[Br:1][C:2]1[C:6]([N:7]([CH3:9])[CH3:8])=[C:5]([C:23]2[CH:24]=[CH:25][C:20]([Cl:19])=[CH:21][CH:22]=2)[S:4][C:3]=1[C:11]([O:13][CH2:14][CH3:15])=[O:12]
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 702EthanolHCID 11430Potassium CarbonateHCID 742994-Chlorophenylboronic acidHCID 68286493HCID 68286493、化合物2 回

生成物 1

HCID 68285965HCID 68285965、化合物収率 76.6%

試薬・触媒・溶媒 2

HCID 178418397
HCID 178418397、化合物
触媒
HCID 1140Toluene溶媒

反応条件

温度
25 °C

実験手順

To a solution of Ethyl 3,5-dibromo-4-(dimethylamino)thiophene-2-carboxylate (compound 34c, 3.0 g, 8.40 mmol) in a mixture of toluene:ethanol (5 ml:30 ml) was added (4-chlorophenyl)boronic acid [1.44 g, 9.24 mmol] and potassium carbonate (2.32 g, 16.80 mmol) at 25° C. Nitrogen gas was bubbled through the reaction mixture for 15 minutes. To the reaction mixture was then added tetrakis(triphenylphosphine)palladium(0) (0.48 g, 0.42 mmol) under nitrogen atmosphere and the reaction mixture was heated at about 95 to 100° C. for 3 hr under stirring. The progress of the reaction was monitored by TLC. The reaction mixture was then cooled to 25° C. and filtered through celite, the celite cake was then washed with ethyl acetate (50 ml). The filtrate so obtained was then concentrated under reduced pressure to obtain a crude product, which was then purified by flash column chromatography using 12% ethyl acetate in hexanes as an eluent to obtain the title compound (2.5 g, 76.56%).

後処理

  1. customNitrogen gas was bubbled through the reaction mixture for 15 minutes
  2. filtrationfiltered through celite
  3. washthe celite cake was then washed with ethyl acetate (50 ml)
  4. customThe filtrate so obtained
  5. concentrationwas then concentrated under reduced pressure
  6. customto obtain a crude product, which
  7. customwas then purified by flash column chromatography

出典と根拠

ORDレコード
ord-20a01a3f64d34b3b95bb2442aa4d2e70
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09393247B2

反応ノート

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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