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5-(Tributylstannyl)-2-(triisopropylsilyl)-1,3-oxazole → N-[6-(1,3-oxazol-5-yl)-5-pyridin-4-ylpyrazin-2-yl]cyclopropanecarboxamide

HRID 1710700
ノート
印刷プレビュー

反応式

HRID 1710700 の反応式
Cl[C:2]1[N:7]=[C:6]([NH:8][C:9]([CH:11]2[CH2:13][CH2:12]2)=[O:10])[CH:5]=[N:4][C:3]=1[C:14]1[CH:19]=[CH:18][N:17]=[CH:16][CH:15]=1.C([Sn](CCCC)(CCCC)[C:25]1[O:29][C:28]([Si](C(C)C)(C(C)C)C(C)C)=[N:27][CH:26]=1)CCC>C1(C)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>[O:29]1[C:25]([C:2]2[N:7]=[C:6]([NH:8][C:9]([CH:11]3[CH2:13][CH2:12]3)=[O:10])[CH:5]=[N:4][C:3]=2[C:14]2[CH:19]=[CH:18][N:17]=[CH:16][CH:15]=2)=[CH:26][N:27]=[CH:28]1
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

5

反応物 2

HCID 114971955-(Tributylstannyl)-2-(triisopropylsilyl)-1,3-oxazoleHCID 59457608N-(6-Chloro-5-pyridin-4-ylpyrazin-2-yl)cyclopropanecarboxamide

生成物 1

HCID 53325341N-[6-(1,3-oxazol-5-yl)-5-pyridin-4-ylpyrazin-2-yl]cyclopropanecarboxamide収率 35%

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒
HCID 7237
O-Xylene
溶媒

反応条件

温度
90 °C

実験手順

A mixture of N-(6-chloro-5-pyridin-4-ylpyrazin-2-yl)cyclopropanecarboxamide (100 mg, 0.36 mmol) and 5-(tributylstannyl)-2-(triisopropylsilyl)-1,3-oxazole (397 mg, 0.73 mmol) in xylene (3 mL) was degassed with argon. The catalyst Pd(PPh3)4 (25 mg, 0.022 mmol, 6 mol %) was added and degassing was repeated. The mixture was heated to 90° C. in a sealed tube and stirred overnight. The mixture was cooled and ethyl acetate and HCl 2N were added. The aqueous layer was washed with ethyl acetate and then neutralized with 6N NaOH. The cloudy solution was extracted with CH2Cl2. The organic layer was dried and concentrated. The residue was purified by flash silica gel chromatography (dichloromethane/methanol 95:5) to give the title compound (36 mg, 35%) as a white solid.

後処理

  1. customwas degassed with argon
  2. customdegassing
  3. temperatureThe mixture was cooled
  4. additionethyl acetate and HCl 2N were added
  5. washThe aqueous layer was washed with ethyl acetate
  6. extractionThe cloudy solution was extracted with CH2Cl2
  7. customThe organic layer was dried
  8. concentrationconcentrated
  9. customThe residue was purified by flash silica gel chromatography (dichloromethane/methanol 95:5)

出典と根拠

ORDレコード
ord-526f9712a73f41bea9e7839067aa4219
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07790728B2

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