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Potassium Carbonate → HCID 86689303、化合物

HRID 1852489
ノート
印刷プレビュー

反応式

HRID 1852489 の反応式
O([C:9]1[CH:18]=[CH:17][C:16]2[CH2:15][CH2:14][CH2:13][CH2:12][C:11]=2[C:10]=1[N+:19]([O-:21])=[O:20])S(C(F)(F)F)(=O)=O.[NH2:22][C:23]1[CH:24]=[C:25]([CH:28]=[CH:29][CH:30]=1)[C:26]#[N:27].C(=O)([O-])[O-].[K+].[K+].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)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.C1(C)C=CC=CC=1>[N+:19]([C:10]1[C:11]2[CH2:12][CH2:13][CH2:14][CH2:15][C:16]=2[CH:17]=[CH:18][C:9]=1[NH:22][C:23]1[CH:24]=[C:25]([CH:28]=[CH:29][CH:30]=1)[C:26]#[N:27])([O-:21])=[O:20]
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 11430Potassium CarbonateHCID 11776TriphenylphosphineHCID 167023-AminobenzonitrileHCID 86689304HCID 86689304、化合物

生成物 1

HCID 86689303HCID 86689303、化合物収率 86.1%

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
110 °C

実験手順

An anhydrous toluene (30 mL) suspension of 1-nitro-5,6,7,8-tetrahydronaphthalen-2-yl triflate (1.95 g, 6.00 mmol), 3-aminobenzonitrile (1.06 g, 9.00 mmol), potassium carbonate (830 mg, 6.00 mmol), tetrakis(triphenylphosphine)palladium (346 mg, 0.30 mmol), and triphenylphosphine (158 mg, 0.60 mmol) was stirred at 110° C. for 18 hours. The reaction mixture was cooled on standing, and filtered. The filtrate was diluted with ethyl acetate. The obtained organic solution was washed with purified water, and dried over anhydrous sodium sulfate. The solvent was removed by evaporation under reduced pressure. The residue was purified by silica gel column chromatography (chloroform) to give the titled compound as orange powder (1.515 g, yield 86%).

後処理

  1. temperatureThe reaction mixture was cooled
  2. filtrationfiltered
  3. additionThe filtrate was diluted with ethyl acetate
  4. washThe obtained organic solution was washed with purified water
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was removed by evaporation under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (chloroform)

出典と根拠

ORDレコード
ord-3cb108f9fb234edaa689835b2f26916f
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08962613B2

反応ノート

読み込み中…

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